A kind of negative electrode material and its preparation method and sodium ion secondary battery
A negative electrode material and ion technology, applied in the field of sodium ion secondary battery, negative electrode material and its preparation, 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
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[0029] The present invention also provides a preparation method of the material described in the above technical solution, comprising the following steps:
[0030] (1) mix calcium salt, phosphate, organic titanium salt and carbon source with water, react to obtain 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 the negative electrode material.
[0033] The invention mixes calcium salt, phosphate, organic titanium salt and carbon source with water, and reacts to obtain the mixture gel. In the present invention, the molar ratio of Ca, P, Ti and C in the mixture gel is preferably 0.5-1.5:5-7:3-5:10-14, more preferably 0.8-1.2:5.5-6.5 :3.5~4.5:11~13, most preferably 1~1.1:6~6.2:4~4.2:11.5~12.5. In the present invention, the concentration of the carbon source in water is preferably 0.015-0.025 mol / L. The present invention has no special...
Embodiment 1
[0059] Dissolve 0.001mol calcium carbonate, 0.006mol ammonium dihydrogen phosphate and 0.004mol isopropyl titanate in 100ml of 0.02mol / L citric acid solution, heat and stir at a constant temperature of 70°C until the solution presents a paste-like gel, and obtain mixture gel;
[0060] Put the mixture gel in a drying oven at 100°C for 12 hours, grind it into a mixture powder in an agate mortar, pre-sinter the mixture powder to 350°C under the protection of nitrogen, keep it warm for 7 hours, take it out after natural cooling, and get Mixture precursor;
[0061] The mixture precursor was pressed into a tablet under a pressure of 22MPa, and the sheet-shaped precursor was sintered to 750°C under the protection of nitrogen and kept for 15 hours. After natural cooling, it was taken out to obtain a negative electrode material for a sodium ion secondary battery.
[0062] An X-ray powder diffraction test was performed on the negative electrode material prepared in this embodiment usin...
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 evenly coated on a copper foil substrate to obtain an electrode sheet;
[0067] After drying the obtained electrode sheet in a vacuum oven at 120°C for 10 hours, press it under a pressure of 20 MPa, and then cut the prepared electrode sheet into thin slices with a size of 8 mm × 8 mm as electrodes, and each thin slice contains 1.7 mg left and right anode materials.
[0068] Use a pure sodium sheet as the counter electrode of the half-cell (a disc with a diameter of about 1cm and a thickness of about 3mm), with sodium perchlorate containing 1mol / L as the solute, dissolved in PC:EC=1:1(v / v ) The organic liquid prepared by the mixed solvent is the electrolyte, and GLASSMICROFIBER FILTERS GF / C TM The separators were assembled into experimental cells in an argon-filled glove box (water and oxygen content less tha...
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