Material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate
Technical field
The present invention relates to the anode material for lithium-ion batteries technical field, be specifically related to the method that material by wet type mixing-two single-step solid phase reaction prepares the modification lithium manganate.
Background technology
Advantages such as lithium ion battery is high with its WV, energy density is big, good cycle, self-discharge are little, memory-less effect.Be widely used in fields such as portable Move tool, digital product, man-made satellite, aerospace at present, also had boundless prospect in fields such as electric bicycle and automobiles.
The method of suitability for industrialized production lithium manganate mainly is a high temperature solid-state method at present.For solid-phase synthesis, the degree of uniformity of raw materials mix and particle size are the important factors that influences the synthetic performance of material, so different mixing methods may have certain influence to the degree of mixing of material and the performance of size-grade distribution and synthetic product.
Summary of the invention
Deficiency to the prior art existence; Technical problem to be solved by this invention is; Provide a kind of and can the enhanced granule surfactivity make it produce the method that material by wet type mixing-two single-step solid phase reaction that many fresh interfaces help ion migration prepares the modification lithium manganate, this method reduces reactant granularity difference, improves the homogeneity of material mixing; Promote the generation of solid state reaction, improve the chemical property of material.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: a kind of material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate, may further comprise the steps:
(1), puts into agitated ball mill according to proportioning weighing Quilonum Retard and white lake;
(2), adding an amount of water in the ball mill starts and stirs the beginning ball milling;
(3), after the granularity of treating Quilonum Retard is ground to certain requirement, adds electrolytic manganese dioxide by proportioning and continue to stir for some time;
(4), blowing, it is dry that material is put into baking oven;
(5), after the completion to be dried, separate broken and granulation, put into atmosphere furnace and once calcine with tablets press;
(6), the material after will once calcining separate broken, carry out the replenishing of lithium after, secondary clacining.
Above-mentioned material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate, and each reactant quality proportioning is 728: 101: 3192.
Above-mentioned material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate, and amount of water is 600ml.
Above-mentioned material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate, and adding electrolytic manganese dioxide continuation churning time is 30min.
Above-mentioned material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate, and granulation is that the Z 150PH (PVA) with 3% is made tackiness agent, and moisture content 18% in the material, and drying temperature is 150 ℃.
Above-mentioned material by wet type mixing-two single-step solid phase reaction prepares the method for modification lithium manganate; Once calcining is in 1h, to be warming up to 350 ℃ from room temperature, under this temperature, is incubated 4h, in 1h, rises to 930 ℃ of insulation 5h again; 2h reduces to 650 ℃ of insulation 15h then, last cooling naturally; Secondary clacining is to lower the temperature naturally after in 2h, rising to 650 ℃ of insulation 26h.
The advantage that material by wet type mixing of the present invention-two single-step solid phase reaction prepares the method for modification lithium manganate is: adopt the mode that adds the water material by wet type mixing; Improved the degree that mixes of material greatly; Make reactant granularity difference reduce, adopt the mode of secondary clacining, effectively strengthened granule surface activity and made it produce the homogeneity that method for mixing that many fresh interfaces help ion migration has improved material mixing; Thereby promoted the generation of solid state reaction, improved the chemical property of material.
Description of drawings
Fig. 1 is the SEM figure of material by wet type mixing modification lithium manganate;
Fig. 2 is the XRD figure of material by wet type mixing modification lithium manganate;
Fig. 3 is a material by wet type mixing modification lithium manganate battery cycle characteristics graphic representation;
Fig. 4 is the first charge-discharge graphic representation of material by wet type mixing modification lithium manganate.
Embodiment
Below in conjunction with specific embodiment the present invention is explained further details;
Embodiment 1:
(1) weighing 693g Quilonum Retard 101g white lake is poured in the agitated ball mill.
(2) adding 600ml water begins to stir.
When (3) Quilonum Retard is ground to about D50 and is 0.6um, add electrolytic manganese dioxide 3192g, continue to stir blowing behind the 30min.
(4) separate broken in the automatic granulating machine and carry out granulation, moisture content 18% pouring into behind the dry materials with 3% Z 150PH.
(5) after 150 ℃ of dryings, carry out particle once sintered.
(6) after the once sintered completion particle is separated brokenly, is added Quilonum Retard 35g, mix and carry out secondary clacining, final powder product.
(7) powder is done XRD, SEM and electrical property analytical test, result such as Fig. 1-shown in Figure 4.
Embodiment 2:
(1) weighing 728g Quilonum Retard 101g white lake is poured in the agitated ball mill.
(2) adding 600ml water begins to stir.
When (3) Quilonum Retard is ground to about D50 and is 0.6um, add electrolytic manganese dioxide 3192g, continue to stir blowing behind the 20min.
(4) separate broken in the automatic granulating machine and carry out granulation, moisture content 16% pouring into behind the dry materials with 3% Z 150PH.
(5) after 150 ℃ of dryings, carry out particle once sintered.
(6) after the once sintered completion particle is separated brokenly, is carried out secondary clacining, final powder product.
(7) powder is done analytical test.
Embodiment 3:
(1) weighing 693g Quilonum Retard 101g white lake is poured in the agitated ball mill.
(2) adding 600ml water begins to stir.
When (3) Quilonum Retard is ground to about D50 and is 0.6um, add electrolytic manganese dioxide 3192g, continue to stir blowing behind the 5min.
(4) separate broken in the automatic granulating machine and carry out granulation, moisture content 16% pouring into behind the dry materials with 3% Z 150PH.
(5) after 150 ℃ of dryings, carry out particle once sintered.
(6) after the once sintered completion particle is separated brokenly, is added Quilonum Retard 35g, mix and carry out secondary clacining, final powder product.
(7) powder is done analytical test.
Certainly, above-mentioned explanation is not to be limitation of the present invention, and the present invention also is not limited to above-mentioned giving an example; Those skilled in the art; In essential scope of the present invention, the variation of making, remodeling, interpolation or replacement all should belong to protection scope of the present invention.