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Negative electrode material as well as preparation method thereof, and sodium ion secondary battery

A negative electrode material and ion technology, applied in the field of negative electrode materials and its preparation, and sodium ion secondary batteries, can solve the problems of not being well applied, limited specific capacity, volume expansion, etc., and achieve excellent reversible specific capacity and good cycle Effect of performance and high specific capacity

Active Publication Date: 2016-10-12
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with positive electrode materials, the study of negative electrode materials is greatly limited, because the radius of sodium ions is about 1.3 times that of lithium ions, which makes some negative electrode materials widely used in lithium-ion batteries can not be well obtained in sodium-ion batteries Applications
Although some carbon-based materials have the ability to store sodium, the specific capacity is very limited, such as the sodium storage specific capacity of amorphous carbon is about 121 mAh / g, and the sodium storage specific capacity of reduced graphene oxide is about 175 mAh / g
At the same time, the discharge platform of carbon-based materials is very low, close to the deposition potential of metallic sodium, resulting in dendrites during charge and discharge, causing safety issues
In addition, the sodium storage properties of some electrode materials (Sn, Sb, P, S, etc.) based on alloying reactions and conversion reactions have also been studied. Rapid expansion occurs, so that the specific capacity decreases, limiting their application

Method used

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  • Negative electrode material as well as preparation method thereof, and sodium ion secondary battery
  • Negative electrode material as well as preparation method thereof, and sodium ion secondary battery
  • Negative electrode material as well as preparation method thereof, and sodium ion secondary battery

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preparation example Construction

[0029] The present invention also provides a method for preparing the material described in the above technical solution, which includes the following steps:

[0030] (1) Mix calcium salt, phosphate, organic titanium salt and carbon source with water, and react to obtain a mixture gel;

[0031] (2) Pre-sintering the mixture gel obtained in the step (1) to obtain a mixture precursor;

[0032] (3) Sintering the mixture precursor obtained in the step (2) to obtain a negative electrode material.

[0033] In the present invention, calcium salt, phosphate, organic titanium salt and carbon source are mixed with water and reacted to obtain a mixture gel. In the present invention, the molar ratio of Ca, P, Ti and C in the mixed gel is preferably 0.5 to 1.5: 5 to 7: 3 to 5: 10 to 14, more preferably 0.8 to 1.2: 5.5 to 6.5 : 3.5 to 4.5: 11 to 13, most preferably 1 to 1.1: 6 to 6.2: 4 to 4.2: 11.5 to 12.5. In the present invention, the concentration of the carbon source in water is preferably 0...

Embodiment 1

[0059] Dissolve 0.001 mol of calcium carbonate, 0.006 mol of ammonium dihydrogen phosphate and 0.004 mol of isopropyl titanate in 100 ml of a 0.02 mol / L citric acid solution, and heat and stir at a constant temperature of 70°C until the solution shows a paste-like gel. Mixture gel

[0060] The mixture gel was dried in a drying box at 100°C for 12 hours and then ground into a mixture powder in an agate mortar. The mixture powder was pre-sintered to 350°C under the protection of nitrogen and kept for 7 hours. After natural cooling, it was taken out. Mixture precursor

[0061] The mixture precursor was pressed into tablets under a pressure of 22 MPa, and the flake precursors were sintered to 750° C. under the protection of nitrogen and kept for 15 hours. After natural cooling, they were taken out to obtain the negative electrode material of the sodium ion secondary battery.

[0062] A Bruker D8 diffractometer equipped with a copper target X-ray tube was used to perform an X-ray powder ...

Embodiment 2

[0066] The negative electrode material prepared in Example 1, acetylene black and PVDF (polyvinylidene fluoride) were mixed into a slurry according to a ratio of 7:2:1, and uniformly coated on the copper foil substrate to obtain an electrode sheet;

[0067] The obtained electrode sheet was dried in a vacuum oven at 120°C for 10 hours, and then compressed under a pressure of 20 MPa, and then the prepared electrode sheet was cut into 8mm×8mm sheets as electrodes, each sheet containing 1.7mg Left and right anode material.

[0068] Use pure sodium tablets as the counter electrode of the half-cell (a disc with a diameter of about 1cm and a thickness of about 3mm), with 1mol / L sodium perchlorate as the solute, dissolved in PC:EC=1:1(v / v ) The organic liquid in the mixed solvent configuration is the electrolyte, which is compatible with the GLASS MICROFIBER FILTERS GF / C TM The diaphragm was assembled into an experimental battery in a glove box filled with argon (water and oxygen content...

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Abstract

The invention provides a negative electrode material as well as a preparation method thereof, and a sodium ion secondary battery. The negative electrode material provided by the invention is made by compounding materials Ca0.5Ti2(PO4)3 comprising a sodium fast ion structure with carbon; as Ca0.5Ti2(PO4)3 with the sodium fast ion structure is provided with more vacancies, more sodium ions can be embedded in a charging / discharging process, and a higher specific capacity can be obtained; carbon compounding can greatly accelerate the transmission of an electron in an individual particle or between a plurality of particles, so that an excellent reversible specific capacity and good cycling performance can be obtained. The sodium ion secondary battery prepared from the negative electrode material provided by the invention can charge or discharge in a voltage interval of 3-0.01 V, the first discharge specific capacity is 463.9 mAh / g, the charge specific capacity is 235.2 mAh / g, and the retention rate of the discharge specific capacity after 30 cycling is as high as 99%.

Description

Technical field [0001] The invention relates to the technical field of functional materials, in particular to a negative electrode material and a preparation method thereof and a sodium ion secondary battery. Background technique [0002] At present, as a secondary energy system, lithium-ion batteries have developed from small electronic devices to high-energy density and high-power power systems. However, the raw materials and cost of lithium-ion batteries still limit its further widespread application in the future to a certain extent. In recent years, due to the increasing demand for low-cost and environmentally friendly energy storage devices, sodium ion batteries have received attention and in-depth research. [0003] An important part that determines the development of sodium ion batteries is the selection of sodium insertion / sodium removal materials. Compared with cathode materials, the research of anode materials is greatly restricted, because the radius of sodium ions is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054
CPCH01M4/366H01M4/5825H01M4/625H01M10/054Y02E60/10
Inventor 杜菲魏芷宣孟醒魏英进王春忠陈岗
Owner JILIN UNIV
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