CN110429324A - A kind of preparation method of the modified compound lithium cell of high capacity - Google Patents
A kind of preparation method of the modified compound lithium cell of high capacity Download PDFInfo
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- CN110429324A CN110429324A CN201910716855.7A CN201910716855A CN110429324A CN 110429324 A CN110429324 A CN 110429324A CN 201910716855 A CN201910716855 A CN 201910716855A CN 110429324 A CN110429324 A CN 110429324A
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Abstract
The present invention settles sth. according to policy or law the preparation method of the modified compound lithium cell of high capacity a kind of, comprising the following steps: the preparation of S1, composite positive pole;The preparation of S2, modified negative electrode material;The preparation of S3, battery positive pole piece;The preparation of S4, negative pole piece of battery;S5, the modified compound lithium cell of high capacity is prepared, the present invention prepares carbon nanotube lithium titanate sulphur composite positive pole using in-situ hydrolysis and melting diffusion technique, it and using the composite material is anode, the modified LTO material of lithium magnesium silicate as cathode, it is prepared into lithium cell, lithium titanate and sulphur are each provided with high capacity as a positive electrode active material, circulating battery stability is significantly improved, lithium magnesium silicate intermediate ion diffusion admittance and its cation exchange capacity (CEC) improve lithium ion transmission efficiency and reduce polarization, are conducive to the holding of battery capacity and stablize play.
Description
Technical field
The invention belongs to lithium cell art fields, and in particular to a kind of preparation method of the modified compound lithium cell of high capacity.
Background technique
The advantages of conductive good, capacity of traditional anode material for lithium-ion batteries is played stably, but theoretical ratio
Capacity is relatively low, is not able to satisfy the demand of the following power and energy-storage system.Sharp crystal form lithium titanate (LTO) is as a kind of common lithium
Ion electrode materials have good cyclical stability, and in lithium-sulfur cell, lithium titanate has the energy of constraint polysulfide shuttle
Power;
However, can be seen that lithium titanate as active material from the charge and discharge platform and cyclic voltammetric testing result of battery
Battery capacity is not improved, still only a kind of additive for electrode, sulphur are only the source of battery capacity, by the lithium of low theoretical capacity
Ion electrode materials are combined with the sulphur of high theoretical capacity, can obtain the common capacity contribution of two various electrode materials;
LTO material has the significant advantages such as safe and stable and environmental-friendly, still, LTO material remain unchanged there is
Many disadvantages, electronic conductivity is poor, and lithium ion diffusion velocity is moderate, greatlys restrict its filling under high current density
Discharge performance, although oneself is through improving the high rate capability of lithium titanate using various method of modifying, many methods are not appropriate for
Therefore industrialization large-scale production it is compound to seek a kind of high capacity modification with excellent high rate capability, stable cycle performance
Lithium cell solves the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of the modified compound lithium cell of high capacity, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the invention provides the following technical scheme: a kind of preparation of the modified compound lithium cell of high capacity
Method, comprising the following steps:
The preparation of S1, composite positive pole:
(1), carbon nanotube ultrasonic disperse the preparation of carbon nanotube lithium titanate composite material: is formed into carbon in dehydrated alcohol
The suspended dispersion liquid of nanometer, LiOH aqueous solution is added into the suspended dispersion liquid of carbon nanometer, obtains the carbon with LiOH after mixing evenly
The solvent of the suspended dispersion liquid of nanometer, after stirring is warming up to 80 DEG C, by TiO (C4H9)4Alcoholic solution is gradually dropped the band quickly stirred
Have in the solvent of the suspended dispersion liquid of carbon nanometer of LiOH, sufficiently after reaction, with 60 DEG C to be evaporated the carbon nanometer with LiOH suspended
The solvent of dispersion liquid is rising to 800 DEG C of heat preservation sintering 2h under an argon atmosphere with the heating rate of 5 DEG C/min, is obtaining carbon nanometer
Pipe lithium titanate composite material;
(2), carbon nanotube lithium titanate composite material the preparation of carbon nanotube lithium titanate sulphur composite positive pole: is instilled into S/
It in CS2 solution, is evaporated, is transferred in tube furnace under room temperature, be sintered 18-22h under 155 DEG C of argon atmospheres, obtain carbon nanotube
Lithium titanate sulphur composite positive pole;
The preparation of S2, modified negative electrode material:
(1), the preparation of pure LTO: hydroxide Where is soluble in water and used with magnetic stirrer, then by butyl titanate
Dehydrated alcohol is diluted, and the butyl titanate after dilution is added drop-wise in lithium hydroxide aqueous solution, is stirred continuously simultaneously, is added dropwise
Continue to stir 30-50min after the completion, the solution mixed is put into 105 DEG C of baking oven and is dried, after being completely dried, sample
With 700-800 DEG C of sintering 5-6h in sintering furnace, pure LTO can be obtained;
(2), the preparation of the modified LTO of lithium magnesium silicate: water is added into lithium magnesium silicate, is formed uniformly in 60 DEG C of stirred in water bath
Colloid, then pure LTO powder is added into colloid, it is stirred 30-50min, is then placed in 105-115 DEG C of baking oven and dries,
Material after drying is sintered 5-6h at 650-750 DEG C, can be obtained the modified LTO of lithium magnesium silicate, that is, obtains modified cathode material
Material;
The preparation of S3, battery positive pole piece: by carbon nanotube lithium titanate sulphur composite positive pole, conductive carbon and polyacrylic acid
It is added in mortar, appropriate N-Methyl pyrrolidone is added after the 30-40min that dry grinds, with scraper by slurry after being fully ground uniformly
Be coated uniformly on aluminium foil with coating machine, the dry 1d in 50 DEG C of baking ovens, the anode pole piece after drying is made, by after drying just
Pole pole piece is washed into anode pole piece of the sequin as battery that diameter is 14m;
The preparation of S4, negative pole piece of battery: modified negative electrode material, conductive carbon and polyacrylic acid are added in mortar,
Appropriate N-Methyl pyrrolidone is added after dry grinding 30-40min, is uniformly applied slurry with coating machine with scraper after being fully ground uniformly
It overlays on aluminium foil, the cathode pole piece after drying is washed into diameter by the dry 1d in 50 DEG C of baking ovens, the cathode pole piece after drying is made
For cathode pole piece of the sequin as battery of 14m;
S5, the modified compound lithium cell of high capacity is prepared: in the glove box of high argon atmospher, by anode pole piece, cathode pole piece
It is assembled together with diaphragm, is wound into core, obtain the modified compound lithium cell of high capacity.
Preferably, the outer diameter of carbon nanotube is 10-20nm in the step S1, length is 50 μm.
Preferably, TiO (C in the step S14H9)4Alcoholic solution be Li and Ti according to the mass ratio of the material be 4:5 prepare
It forms.
Preferably, the mass concentration of S/CS2 solution is 10mg/mL in the step S1.
Preferably, carbon nanotube lithium titanate sulphur composite positive pole in the step S3, conductive carbon and polyacrylic acid matter
Amount is than being 8:1:1.
Preferably, the amount of coating machine coating substance is 1mg/cm in the step S32。
Preferably, the mass ratio of negative electrode material modified in the step S4, conductive carbon and polyacrylic acid is 8:1:1.
Preferably, the amount of coating machine coating substance is similarly 1mg/cm in the step S42。
Technical effect and advantage of the invention: the preparation method of the modified compound lithium cell of the high capacity utilizes in-situ hydrolysis
Carbon nanotube lithium titanate sulphur composite positive pole is prepared with melting diffusion technique, and is anode, lithium magnesium silicate with the composite material
Modified LTO material is cathode, is prepared into lithium cell, in battery charge and discharge process, as a positive electrode active material by lithium titanate and sulphur
It is each provided with high capacity, circulating battery stability is significantly improved, and uniform lithium magnesium silicate clad can inhibit crystal grain to reunite
With grow up, lithium magnesium silicate can improve the electronic conductivity and ionic conductivity of electrolyte, and table silicon ion and magnesium ion are co-doped with
Miscellaneous to improve electronic conductivity, lithium magnesium silicate intermediate ion diffusion admittance and its cation exchange capacity (CEC) improve lithium ion transmission efficiency
And polarization is reduced, anode pole piece and cathode pole piece are assembled into all solid state lithium battery, provide high safety, high-energy density
Solid lithium battery system, lithium titanate provide capacity, improve positive active material content, while fettering polysulfide, subtract
Small shuttle is answered, and is conducive to the holding of sulfur capacity and stablizes play.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
A kind of preparation method of the modified compound lithium cell of high capacity, comprising the following steps:
The preparation of S1, composite positive pole:
(1), carbon nanotube ultrasonic disperse the preparation of carbon nanotube lithium titanate composite material: is formed into carbon in dehydrated alcohol
The suspended dispersion liquid of nanometer, LiOH aqueous solution is added into the suspended dispersion liquid of carbon nanometer, obtains the carbon with LiOH after mixing evenly
The solvent of the suspended dispersion liquid of nanometer, after stirring is warming up to 80 DEG C, by TiO (C4H9)4Alcoholic solution is gradually dropped the band quickly stirred
Have in the solvent of the suspended dispersion liquid of carbon nanometer of LiOH, sufficiently after reaction, with 60 DEG C to be evaporated the carbon nanometer with LiOH suspended
The solvent of dispersion liquid is rising to 800 DEG C of heat preservation sintering 2h under an argon atmosphere with the heating rate of 5 DEG C/min, is obtaining carbon nanometer
Pipe lithium titanate composite material;
(2), carbon nanotube lithium titanate composite material the preparation of carbon nanotube lithium titanate sulphur composite positive pole: is instilled into S/
It in CS2 solution, is evaporated, is transferred in tube furnace under room temperature, be sintered 18-22h under 155 DEG C of argon atmospheres, obtain carbon nanotube
Lithium titanate sulphur composite positive pole;
The preparation of S2, modified negative electrode material:
(1), the preparation of pure LTO: hydroxide Where is soluble in water and used with magnetic stirrer, then by butyl titanate
Dehydrated alcohol is diluted, and the butyl titanate after dilution is added drop-wise in lithium hydroxide aqueous solution, is stirred continuously simultaneously, is added dropwise
Continue to stir 30-50min after the completion, the solution mixed is put into 105 DEG C of baking oven and is dried, after being completely dried, sample
With 700-800 DEG C of sintering 5-6h in sintering furnace, pure LTO can be obtained;
(2), the preparation of the modified LTO of lithium magnesium silicate: water is added into lithium magnesium silicate, is formed uniformly in 60 DEG C of stirred in water bath
Colloid, then pure LTO powder is added into colloid, it is stirred 30-50min, is then placed in 105-115 DEG C of baking oven and dries,
Material after drying is sintered 5-6h at 650-750 DEG C, can be obtained the modified LTO of lithium magnesium silicate, that is, obtains modified cathode material
Material;
The preparation of S3, battery positive pole piece: by carbon nanotube lithium titanate sulphur composite positive pole, conductive carbon and polyacrylic acid
It is added in mortar, appropriate N-Methyl pyrrolidone is added after the 30-40min that dry grinds, with scraper by slurry after being fully ground uniformly
Be coated uniformly on aluminium foil with coating machine, the dry 1d in 50 DEG C of baking ovens, the anode pole piece after drying is made, by after drying just
Pole pole piece is washed into anode pole piece of the sequin as battery that diameter is 14m;
The preparation of S4, negative pole piece of battery: modified negative electrode material, conductive carbon and polyacrylic acid are added in mortar,
Appropriate N-Methyl pyrrolidone is added after dry grinding 30-40min, is uniformly applied slurry with coating machine with scraper after being fully ground uniformly
It overlays on aluminium foil, the cathode pole piece after drying is washed into diameter by the dry 1d in 50 DEG C of baking ovens, the cathode pole piece after drying is made
For cathode pole piece of the sequin as battery of 14m;
S5, the modified compound lithium cell of high capacity is prepared: in the glove box of high argon atmospher, by anode pole piece, cathode pole piece
It is assembled together with diaphragm, is wound into core, obtain the modified compound lithium cell of high capacity.
Specifically, the outer diameter of carbon nanotube is 10-20nm in the step S1, length is 50 μm.
Specifically, TiO (C in the step S14H9)4Alcoholic solution be Li and Ti according to the mass ratio of the material be 4:5 prepare
It forms.
Specifically, the mass concentration of S/CS2 solution is 10mg/mL in the step S1.
Specifically, the matter of carbon nanotube lithium titanate sulphur composite positive pole in the step S3, conductive carbon and polyacrylic acid
Amount is than being 8:1:1.
Specifically, the amount of coating machine coating substance is 1mg/cm in the step S32。
Specifically, the mass ratio of negative electrode material modified in the step S4, conductive carbon and polyacrylic acid is 8:1:1.
Specifically, the amount of coating machine coating substance is similarly 1mg/cm in the step S42。
The preparation method of the modified compound lithium cell of the high capacity prepares carbon nanometer using in-situ hydrolysis and melting diffusion technique
Pipe lithium titanate sulphur composite positive pole, and be anode, the modified LTO material of lithium magnesium silicate as cathode using the composite material, it is prepared into
Lithium titanate and sulphur in battery charge and discharge process, are each provided with high capacity, circulating battery is steady by lithium cell as a positive electrode active material
Qualitative to be significantly improved, uniform lithium magnesium silicate clad can inhibit crystal grain to reunite and grow up, and lithium magnesium silicate can improve electricity
The electronic conductivity and ionic conductivity of liquid are solved, table silicon ion and magnesium ion codope improve electronic conductivity, magnesium silicate
Lithium intermediate ion diffusion admittance and its cation exchange capacity (CEC) improve lithium ion transmission efficiency and reduce polarization, anode pole piece and
Cathode pole piece is assembled into all solid state lithium battery, provides high safety, high-energy density solid lithium battery system, and lithium titanate mentions
Capacity has been supplied, has improved positive active material content, while fettering polysulfide, has reduced to shuttle and answer, be conducive to the guarantor of sulfur capacity
Hold and stablize performance.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (8)
1. a kind of preparation method of the modified compound lithium cell of high capacity, which comprises the following steps:
The preparation of S1, composite positive pole:
(1), carbon nanotube ultrasonic disperse the preparation of carbon nanotube lithium titanate composite material: is formed into carbon nanometer in dehydrated alcohol
LiOH aqueous solution is added into the suspended dispersion liquid of carbon nanometer for suspended dispersion liquid, obtains the carbon nanometer with LiOH after mixing evenly
The solvent of suspended dispersion liquid, after stirring is warming up to 80 DEG C, by TiO (C4H9)4Alcoholic solution is gradually dropped having of quickly stirring
In the solvent of the suspended dispersion liquid of carbon nanometer of LiOH, sufficiently after reaction, with 60 DEG C at be evaporated suspended point of carbon nanometer with LiOH
The solvent of dispersion liquid is rising to 800 DEG C of heat preservation sintering 2h under an argon atmosphere with the heating rate of 5 DEG C/min, is obtaining carbon nanotube
Lithium titanate composite material;
(2), carbon nanotube lithium titanate composite material the preparation of carbon nanotube lithium titanate sulphur composite positive pole: is instilled into S/CS2
It in solution, is evaporated, is transferred in tube furnace under room temperature, be sintered 18-22h under 155 DEG C of argon atmospheres, obtain carbon nanotube metatitanic acid
Lithium sulphur composite positive pole;
The preparation of S2, modified negative electrode material:
(1), the preparation of pure LTO: hydroxide Where is soluble in water and with magnetic stirrer, then by butyl titanate with anhydrous
Ethyl alcohol is diluted, and the butyl titanate after dilution is added drop-wise in lithium hydroxide aqueous solution, is stirred continuously simultaneously, is added dropwise to complete
After continue stir 30-50min, the solution mixed is put into 105 DEG C of baking oven and is dried, after being completely dried, sample is being burnt
With 700-800 DEG C of sintering 5-6h in freezing of a furnace, pure LTO can be obtained;
(2), the preparation of the modified LTO of lithium magnesium silicate: water is added into lithium magnesium silicate, forms equal spin coating in 60 DEG C of stirred in water bath
Body, then pure LTO powder is added into colloid, it is stirred 30-50min, is then placed in 105-115 DEG C of baking oven and dries, is dried
Material after dry is sintered 5-6h at 650-750 DEG C, can be obtained the modified LTO of lithium magnesium silicate, that is, obtains modified negative electrode material;
The preparation of S3, battery positive pole piece: carbon nanotube lithium titanate sulphur composite positive pole, conductive carbon and polyacrylic acid are added
Into mortar, appropriate N-Methyl pyrrolidone is added after the 30-40min that dry grinds, is applied slurry with scraper after being fully ground uniformly
Cloth machine is coated uniformly on aluminium foil, the dry 1d in 50 DEG C of baking ovens, the anode pole piece after drying is made, by the positive pole after drying
Piece is washed into anode pole piece of the sequin as battery that diameter is 14m;
The preparation of S4, negative pole piece of battery: modified negative electrode material, conductive carbon and polyacrylic acid are added in mortar, dry grinding
Appropriate N-Methyl pyrrolidone is added after 30-40min, is coated uniformly on slurry with coating machine with scraper after being fully ground uniformly
On aluminium foil, the dry 1d in 50 DEG C of baking ovens, the cathode pole piece after drying is made, the cathode pole piece after drying, which is washed into diameter, is
Cathode pole piece of the sequin of 14m as battery;
S5, prepare the modified compound lithium cell of high capacity: in the glove box of high argon atmospher, by anode pole piece, cathode pole piece and every
Film is assembled together, and is wound into core, obtains the modified compound lithium cell of high capacity.
2. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The outer diameter of carbon nanotube is 10-20nm in rapid S1, length is 50 μm.
3. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
TiO (C in rapid S14H9)4Alcoholic solution is being formulated according to the mass ratio of the material for 4:5 for Li and Ti.
4. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The mass concentration of S/CS2 solution is 10mg/mL in rapid S1.
5. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The mass ratio of carbon nanotube lithium titanate sulphur composite positive pole, conductive carbon and polyacrylic acid is 8:1:1 in rapid S3.
6. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The amount of coating machine coating substance is 1mg/cm in rapid S32。
7. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The mass ratio of modified negative electrode material, conductive carbon and polyacrylic acid is 8:1:1 in rapid S4.
8. a kind of preparation method of the modified compound lithium cell of high capacity according to claim 1, it is characterised in that: the step
The amount of coating machine coating substance is similarly 1mg/cm in rapid S42。
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