CN109638248A - A kind of preparation method of porous triple material, porous triple material and half-cell - Google Patents
A kind of preparation method of porous triple material, porous triple material and half-cell Download PDFInfo
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract
The invention discloses a kind of preparation method of porous triple material, porous triple material and half-cells, are related to technical field of lithium ion.This method includes being dried to obtain primary particle after template and presoma are mixed in aqueous solution；It is sintered after primary particle is mixed with lithium source.This method passes through the mixing of presoma and template, it can make in template insertion presoma, change the pattern of presoma to a certain extent, simultaneously and after lithium source mixed sintering, carbon conversion in template flies out for carbon dioxide gas, no pollution to the environment, while the position that original carbon is occupied then is available, and cellular is formed.Cellular ternary material makes the contact area of positive electrode and electrolyte become larger, and contacts more abundant, while shortening the diffusion path of lithium ion, improves the high rate performance of lithium ion battery, the chemical properties such as cycle performance.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of preparation method of porous triple material, more
Hole ternary material and half-cell.
Background technique
Positive electrode is the important component of lithium ion battery, and with layer structure ternary material because of price just
Preferably, the advantages that capacity height, good cycle, higher security performance, it is considered to be the most anode material for lithium-ion batteries of prospect
One of.But ternary material has the shortcomings that, seriously restricts its application development, lot of domestic and foreign scholar, which studies, to attempt to pass through table
Bread covers, adulterates the performance for improving ternary material.But the method for preparing porous triple material is but rarely reported.
Summary of the invention
One of the objects of the present invention is to provide a kind of preparation methods of porous triple material, and this method is simple and convenient, can
Cellular ternary material quickly is prepared, so that the positive electrode of lithium ion battery and the contact area of electrolyte obtain
The electricity such as high rate performance, the cycle performance for improving significantly, while shortening the diffusion path of lithium ion, and then improve lithium ion battery
Chemical property.
The second object of the present invention is to provide a kind of porous triple material, which passes through above-mentioned porous
The preparation method of ternary material is prepared.The porous triple material may make the positive electrode and electrolyte of lithium ion battery
Contact area obtains improving significantly, while shortening the diffusion path of lithium ion, and then the high rate performance of raising lithium ion battery,
The chemical properties such as cycle performance.
The third object of the present invention is to provide a kind of half-cell, which is prepared by above-mentioned porous triple material
It obtains.Therefore, the contact area of the half-cell and electrolyte can be obtained improves significantly, so as to shorten the diffusion road of lithium ion
Diameter, and then the chemical properties such as the high rate performance of lithium ion battery, cycle performance can be improved.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of porous triple material comprising:
Spray drying obtains primary particle after template and presoma are mixed in aqueous solution；
It is sintered after primary particle is mixed with lithium source.
The present invention proposes a kind of porous triple material, is prepared by the preparation method of above-mentioned porous triple material
It arrives.
The present invention proposes a kind of half-cell, is prepared by the following method to obtain:
Mixture is obtained after above-mentioned porous triple material, conductive agent and binder are mixed；
Mixture is subjected to ball milling, and the slurry that ball milling obtains successively is coated and is dried in vacuo.
Preparation method, the beneficial effect of porous triple material and half-cell of the porous triple material of the embodiment of the present invention
It is:
The preparation method for the porous triple material that the embodiment of the present invention provides, including by template and presoma water-soluble
Spray drying obtains primary particle after being mixed in liquid；It is sintered after primary particle is mixed with lithium source.Pass through presoma
With the mixing of template, can make to change the pattern of presoma, while and lithium to a certain extent in template insertion presoma
After the mixed sintering of source, the carbon conversion in template flies out for carbon dioxide gas, no pollution to the environment, while original carbon is accounted for
According to position be then available, formed cellular.Cellular ternary material becomes the contact area of positive electrode and electrolyte
Greatly, it contacts more abundant, while shortening the diffusion path of lithium ion, improve the high rate performance of lithium ion battery, cyclicity
The chemical properties such as energy.
The porous triple material that the embodiment of the present invention provides is prepared by the preparation method of above-mentioned porous triple material
It obtains.The porous triple material may make the positive electrode of lithium ion battery and the contact area of electrolyte to obtain mentioning significantly
Height, while the electrochemistries such as high rate performance, cycle performance for shortening the diffusion path of lithium ion, and then improving lithium ion battery
Energy.
The half-cell that the embodiment of the present invention provides, is prepared by above-mentioned porous triple material.It therefore, should half electricity
The contact area of pond and electrolyte can be obtained to be improved significantly, so as to shorten the diffusion path of lithium ion, and then lithium can be improved
The chemical properties such as high rate performance, the cycle performance of ion battery.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is that the SEM of Nano carbon balls provided by the invention schemes；
Fig. 2 is that the SEM of porous triple material provided by the invention schemes；
Fig. 3 is cycle-index-gram volume figure of porous triple material provided by the invention.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The preparation method of the porous triple material of the embodiment of the present invention, porous triple material and half-cell are carried out below
It illustrates.
The embodiment provides a kind of preparation methods of porous triple material comprising:
Spray drying obtains primary particle after template and presoma are mixed in aqueous solution；By primary particle with
It is sintered after lithium source mixing.
In detail, by the mixing of presoma and template, can make in template insertion presoma, to a certain extent
Change the pattern of presoma, while with after lithium source mixed sintering, the carbon conversion in template flies out for carbon dioxide gas, to ring
Border is pollution-free, while the position that original carbon is occupied then is available, and forms cellular.Cellular ternary material makes anode
The contact area of material and electrolyte becomes larger, and contacts more abundant, while shortening the diffusion path of lithium ion, improve lithium from
The high rate performance of sub- battery, the chemical properties such as cycle performance.
As a preferred option, in the present embodiment, template is Nano carbon balls.It, will by the pretreatment to presoma
High temperature sintering, Nano carbon balls are converted into carbon dioxide and fly out after mixing according to a certain percentage with lithium source for it, and originally carbon occupies
Position be then available, form cavernous ternary material, compared with traditional ternary material, the electricity of cellular ternary material
Chemical property improves a lot to a certain extent.
Specifically, Nano carbon balls are prepared by the following method to obtain: glucose solution is reacted in hydrothermal reaction kettle；It will
Product after reaction is centrifuged, and with ethyl alcohol and water washing；Product after washing is dried.
Wherein, in the step of reacting glucose solution in hydrothermal reaction kettle, the concentration of glucose solution is
0.5mol/L, and react parameter be 160 DEG C at a temperature of react 3.5h；The step of product after washing is dried
In, dry temperature is 80 DEG C, and the partial size of the Nano carbon balls after drying is about 200nm.Fig. 1 is Nano carbon balls provided by the invention
SEM figure.Referring to Fig. 1, dispersibility also compares as can be seen that agglomeration do not occur substantially in prepared Nano carbon balls
It is good, spherical rule and (this Nano carbon balls surface for being primarily due to synthesis has-OH and-CO group) uniform in size, diameter
About 200nm.
In detail, in an embodiment of the present invention, presoma may be selected to be 622 type presomas；Also, precursor is
When 622 type presoma, the step of obtaining primary particle is spray-dried after template and presoma are mixed in aqueous solution
It specifically includes:
500 parts of 622 type presomas are weighed according to parts by weight to be dissolved in 2000~3500 parts of deionized water；It is preferred that
3000 parts of deionized water can be selected in ground；
It is stirring evenly and then adding into 35~80 parts of Nano carbon balls, it is preferable that 50 parts of Nano carbon balls can be added, and pass through spray
Mist drying equipment obtains the presoma mixed with Nano carbon balls after being dried, and is 1 mixed with the partial size of the presoma of Nano carbon balls
~20 μm.
Wherein, Fig. 2 is the SEM picture of prepared porous triple material.It can be seen from the figure that prepared porous three
First material is made of many hollow structures, and the edge of hollow hemisphere adheres to many nanoparticles, these nanoparticles are in unformed
The shapes and sizes of state, hollow structure are uniform, and diameter is about 200nm, and roughly equal with the partial size of Nano carbon balls, this shows carbon
Nanosphere plays template in system.
As a preferred option, in the embodiment of invention, lithium source is that lithium hydroxide or lithium carbonate are matched according to default lithium
The lithium source arrived.The step of being sintered after primary particle is mixed with lithium source specifically includes:
Lithium source is weighed with L/M=1.03~1.1 by lithium, it is preferable that L/M=1.05, wherein lithium source is lithium carbonate/hydrogen-oxygen
Change lithium；
Lithium source is sintered with the presoma mixed with Nano carbon balls by planetary ball mill after mixing.
Wherein, presoma and lithium source are not added wet using planetary ball mill progress dry mixed during the preparation process
Method technique, lithium ion are not easy to form Li dendrite in negative terminal surface, ensure that prepared ternary material gram volume with higher.
It is further preferred that in an embodiment of the present invention, sintering be under air or oxygen atmosphere with constant 10 DEG C/
Min is warming up to 300 DEG C, 2~3h of constant temperature, then is warming up to 500 DEG C, 2~3h of constant temperature with constant 10 DEG C/min, finally with constant 10
DEG C/min is warming up to 900 DEG C, natural cooling after 10~12h of constant temperature.Certainly, in other embodiments of the invention, the ginseng of sintering
Number can also be selected and be adjusted according to demand, and the embodiment of the present invention is without limitation.
The porous triple material that the embodiment of the present invention provides is prepared by the preparation method of above-mentioned porous triple material
It obtains.The porous triple material may make the positive electrode of lithium ion battery and the contact area of electrolyte to obtain mentioning significantly
Height, while the electrochemistries such as high rate performance, cycle performance for shortening the diffusion path of lithium ion, and then improving lithium ion battery
Energy.
The half-cell that the embodiment of the present invention provides, is prepared by the following method to obtain:
Mixture is obtained after above-mentioned porous triple material, conductive agent and binder are mixed；
Mixture is subjected to ball milling, and the slurry that ball milling obtains successively is coated and is dried in vacuo.The half-cell with
The contact area of electrolyte can be obtained to be improved significantly, so as to shorten the diffusion path of lithium ion, and then lithium ion can be improved
The chemical properties such as high rate performance, the cycle performance of battery.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of porous triple material is present embodiments provided, is prepared by the following method to obtain:
S1: weighing a certain amount of glucose, is configured to the glucose solution of 0.5moL/L, 160 DEG C in hydrothermal reaction kettle
3.5h is reacted, then a large amount of ethyl alcohol and water washing are used in centrifuge separation, finally drying at 80 DEG C can be obtained partial size and be about
The Nano carbon balls of 200nm；
S2: weighing 622 type presoma 500g and be dissolved in 3000g deionized water, be stirring evenly and then adding into 50g Nano carbon balls,
Then suspension is squeezed into spray drying device by peristaltic pump and is dried, obtain the presoma mixed with Nano carbon balls, institute
The particle size range of product is obtained at 1~20 μm.
S3: lithium source (lithium carbonate/lithium hydroxide) and gained are weighed mixed with the presoma of Nano carbon balls with L/M=1.05 by lithium
It is uniformly mixed by planetary ball mill, obtains product to be burnt.
S4: gained product to be burnt is placed in atmosphere Muffle furnace, with constant 10 DEG C/min liter under air or oxygen atmosphere
Temperature is warming up to 500 DEG C, 2~3h of constant temperature to 300 DEG C, 2~3h of constant temperature, then with constant 10 DEG C/min, finally with constant 10 DEG C/min
900 DEG C, 10~12h of constant temperature are warming up to, natural cooling obtains porous cobalt nickel lithium manganate ternary material.
The present embodiment additionally provides a kind of half-cell, is prepared by the following method to obtain:
S1: the ternary material, conductive agent and binder of preparation are mixed according to a certain percentage；
S2: and then prepare uniformly mixed and modest viscosity slurry with vacuum ball grinder 600rmp ball milling 2h and applied
Electrode slice is prepared in cloth, vacuum drying.
Wherein, conductive agent uses super " P ", and diaphragm is celgard 2300, and electrolyte selects the LiPF6 of 1mol/L to lead
Electric salt and DMC:DEC:EC (wt%)=1:1:1 solvent, suitable VC is added in electrolyte solution and does additive.Charge and discharge
Blanking voltage is 2.3~4.75V, and the first effect and cycle performance of battery are tested under 0.1C state, as a result sees Fig. 3, as can be seen from FIG. 3
The porous triple material gram volume of preparation is high, good cycle, has carried out after 30 circulations capacity retention ratio 94% or more,
Charge and discharge efficiency is up to 95% for the first time.
In conclusion the preparation method for the porous triple material that the embodiment of the present invention provides, this method is simple and convenient, can
Cellular ternary material quickly is prepared, so that the positive electrode of lithium ion battery and the contact area of electrolyte obtain
The electricity such as high rate performance, the cycle performance for improving significantly, while shortening the diffusion path of lithium ion, and then improve lithium ion battery
Chemical property.
The porous triple material that the embodiment of the present invention provides is prepared by the preparation method of above-mentioned porous triple material
It obtains.The porous triple material may make the positive electrode of lithium ion battery and the contact area of electrolyte to obtain mentioning significantly
Height, while the electrochemistries such as high rate performance, cycle performance for shortening the diffusion path of lithium ion, and then improving lithium ion battery
Energy.
The embodiment of the present invention is the half-cell provided, is prepared by above-mentioned porous triple material.Therefore, should
The contact area of half-cell and electrolyte can be obtained to be improved significantly, so as to shorten the diffusion path of lithium ion, and then can be mentioned
The chemical properties such as high rate performance, the cycle performance of high-lithium ion battery.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of porous triple material, characterized in that it comprises:
Spray drying obtains primary particle after template and presoma are mixed in aqueous solution；
It is sintered after the primary particle is mixed with lithium source.
2. the preparation method of porous triple material according to claim 1, it is characterised in that:
The template is Nano carbon balls.
3. the preparation method of porous triple material according to claim 2, it is characterised in that:
The Nano carbon balls are prepared by the following method to obtain:
Glucose solution is reacted in hydrothermal reaction kettle；
Product after reaction is centrifuged, and with ethyl alcohol and water washing；
Product after washing is dried.
4. the preparation method of porous triple material according to claim 3, it is characterised in that:
In the step of reacting the glucose solution in the hydrothermal reaction kettle, the concentration of the glucose solution is
0.5mol/L, and react parameter be 160 DEG C at a temperature of react 3.5h；
In the step of product after washing is dried, dry temperature is 80 DEG C.
5. the preparation method of porous triple material according to any one of claim 2 to 4, it is characterised in that:
The presoma may be selected to be 622 type presomas；
Also, when the presoma is 622 type presoma, the template is mixed in aqueous solution with the presoma and is stirred
The step of primary particle is dried to obtain after mixing specifically includes:
500 parts of 622 type presomas are weighed according to parts by weight to be dissolved in 2000~3500 parts of deionized water；
35~80 parts of Nano carbon balls are stirring evenly and then adding into, and obtain receiving mixed with carbon after being dried by spray drying device
The presoma of rice ball, and the partial size of the presoma mixed with Nano carbon balls is 1~20 μm.
6. the preparation method of porous triple material according to claim 5, it is characterised in that:
The lithium source is that lithium hydroxide or lithium carbonate match obtained lithium source according to default lithium.
7. the preparation method of porous triple material according to claim 6, it is characterised in that:
The step of being sintered after the primary particle is mixed with lithium source specifically includes:
The lithium source is weighed with L/M=1.03~1.1 by lithium, wherein the lithium source is lithium carbonate/lithium hydroxide；
The lithium source is sintered with the presoma mixed with Nano carbon balls by planetary ball mill after mixing.
8. the preparation method of porous triple material according to claim 7, it is characterised in that:
Sintering be warming up to 300 DEG C, 2~3h of constant temperature under air or oxygen atmosphere with constant 10 DEG C/min, then with constant 10 DEG C/
Min is warming up to 500 DEG C, 2~3h of constant temperature, is finally warming up to 900 DEG C with constant 10 DEG C/min, natural cooling after 10~12h of constant temperature.
9. a kind of porous triple material, it is characterised in that:
The porous triple material is prepared by the preparation method of porous triple material described in any item of the claim 1 to 8
It obtains.
10. a kind of half-cell, which is characterized in that the half-cell is prepared by the following method to obtain:
Mixture is obtained after porous triple material as claimed in claim 9, conductive agent and binder are mixed；
The mixture is subjected to ball milling, and the slurry that ball milling obtains successively is coated and is dried in vacuo.
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