CN106082361A - A kind of preparation method of anode material for lithium-ion batteries hollow porous nano/submicron multilevel hierarchy nickel ion doped - Google Patents
A kind of preparation method of anode material for lithium-ion batteries hollow porous nano/submicron multilevel hierarchy nickel ion doped Download PDFInfo
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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Abstract
The present invention relates to the preparation method of a kind of anode material for lithium-ion batteries hollow porous nano/submicron multilevel hierarchy nickel ion doped.Mainly comprise the steps that preparation manganese salt solution and alkaline agent solution respectively, subsequently alkaline agent solution is joined in manganese salt solution, reaction obtains nickel ion doped presoma after terminating, heat treatment 1～10 hours at a temperature of 100～1000 DEG C, mix homogeneously in ethanol with lithium salts and soluble nickel salt again, it is transferred to after drying and grinding in high temperature furnace at a temperature of 500～1000 DEG C heat treatment 1～20 hours, to obtain described high-voltage lithium nickel manganate material.Preparation method technique of the present invention is simple, easily operates, low cost, beneficially industrial volume production.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, be specifically related to one and there is hollow porous nanometer/Asia
The preparation method of the high-voltage lithium nickel manganate anode material of micron multi-stage and the nickel ion doped conduct prepared based on the method
The application of anode material for lithium-ion batteries.
Background technology
The fast development of electric automobile, more and more higher to the performance requirement of lithium ion battery.Current lithium ion battery development
One of trend improves its energy density exactly, ensures to have relatively low price, high heat stability and long circulation longevity simultaneously
Life.The positive electrodes such as traditional cobalt acid lithium, due to expensive, toxicity is bigger so that it is large-scale application is restricted.
Spinel nickel manganate cathode material for lithium is owing to having the high working voltage of 4.7V, three-dimensional lithium ion diffusion admittance, height
Energy density, advantages of environment protection, have become as the most promising anode material for lithium-ion batteries.But nickel ion doped positive pole
Material capacity decay is very fast, and the most in high temperature environments, the capacity attenuation that manganese ion dissolution causes is even more serious.The nucleocapsid of preparation
Structure nickel ion doped only respectively reaches 98% through 30 charge and discharge cycles capability retentions at room temperature 25 DEG C and high temperature 55 DEG C
With 95% (J.Power Sources, 2014,256:66), the nickel ion doped granule of a size of 1-3 micron warp under 55 DEG C of high temperature
Cross 100 charge and discharge cycles and only there is the capability retention (Electrochim.Acta, 2011,56:6554) of 73.1%, micron
The spherical nickel-lithium manganate of size under 55 DEG C of high temperature after 100 circulations conservation rate only up to 55% (J.Power Sources,
2015,281:85).For nickel ion doped, the cycle performance and the high rate performance that obtain excellence remain huge choosing simultaneously
War.
Being found by numerous studies, hollow porous material can provide extra space, and these spaces can subtract effectively
The structural stress produced in light lithium ion insertion/withdrawal process, therefore can improve the cyclical stability of material.Additionally, it is hollow
Loose structure has big specific surface area, has resulted in sufficient reactivity region.Meanwhile, nano level primary material
Material shortens the diffusion length of lithium ion significantly, increases the contact area between electrode and electrolyte and then increases reactivity
Region, thus improve the high rate performance of spinel nickel lithium manganate material, the secondary groups dress body of submicron order can ensure that material
The stability of structure, this special nano/submicron multilevel hierarchy can effectively improve the chemical property of positive electrode.
In sum, hollow porous nano/submicron multilevel hierarchy positive electrode is obtained in that excellent cycling performance and high rate performance.According to
Known to applicant, there is presently no report and there is cube pattern spinel nickel manganese of hollow porous nano/submicron multilevel hierarchy
Acid lithium anode material.After being assembled into battery, cube pattern nickel ion doped of the hollow porous nano/submicron multilevel hierarchy of preparation
There are high rate performance and room temperature 25 DEG C and 55 DEG C of cycle performances of high temperature of excellence: the electric discharge specific volume under 1C, 2C, 3C, 4C and 5C
Amount is respectively 121.4,117.3,114.4,111.3 and 108.1mAh g-1；Through 100 times at room temperature 25 DEG C and high temperature 55 DEG C
Charge and discharge cycles capability retention is up to 99.5% and 98.4% respectively, demonstrates the cycle performance of excellence.
Summary of the invention
The purpose of the present invention with the defect overcoming above-mentioned prior art to exist, it is provided that a kind of convenient, simply, the most energy-conservation
Cube pattern high-voltage lithium nickel manganate positive pole of hollow porous nano/submicron multilevel hierarchy of preparation electrochemical performance
The method of material, hollow porous nano/submicron multilevel hierarchy prepared by the method, it is provided that extra space can subtract effectively
The structural stress produced in light lithium ion insertion/withdrawal process, nano level primary material shortens the expansion of lithium ion significantly
Dissipate distance and big specific surface area, resulted in sufficient reactivity region, thus improve cycle performance and the most forthright
Can, to meet the demand to current lithium ion battery.
The technical scheme of the preparation method of the nickel lithium manganate cathode material of the present invention is as follows:
(1) the soluble manganese salt of certain mass is dissolved in the high purity water of certain volume, then according to high purity water and short chain
Unit alcohol volume ratio is (1～10): 3 are added dropwise over short chain units alcohol, stir a period of time, obtain settled solution A.
(2) alkaline reagent of certain mass is dissolved in high purity water, obtains settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) the nickel ion doped presoma that upper step obtains is put in high temperature furnace at a temperature of 100～1000 DEG C heat treatment 1～
10 hours, it is sufficiently mixed in ethanol with lithium salts and soluble nickel salt subsequently, is then dried under the conditions of 120 DEG C, grinds 30 points
Presoma powder body is obtained after clock.Finally, presoma powder body is transferred in high temperature furnace heat treatment 1 at a temperature of 500～1000 DEG C
～20 hours, cool to room temperature with the furnace and obtain nickel lithium manganate cathode material.
Above-described soluble manganese salt is: manganese chloride, manganese nitrate, manganese acetate, one or more in manganese sulfate
Salt-mixture；Described short chain units alcohol is: ethanol, isopropanol, normal propyl alcohol, n-butyl alcohol, one or more in isobutanol
Mixed solvent；Described alkaline reagent is: carbamide, sodium hydroxide, ammonia, one or more the mixing in ammonium hydrogen carbonate
Alkali；Described lithium salts is: Quilonorm (SKB), lithium carbonate, Lithium hydrate, one or more mixing lithium salts of lithium nitrate；Described solvable
Property nickel salt is: Nickel dichloride., nickel nitrate, nickel acetate, one or more the salt-mixture in nickel sulfate.
Cube pattern high voltage nickel mangaic acid of the hollow porous nano/submicron multilevel hierarchy obtained produced according to the present invention
Lithium anode material pattern is homogeneous, better crystallinity degree, is a kind of cycle performance and the excellent anode material for lithium-ion batteries of high rate performance.
In addition, low cost of the present invention, process route is simple, and energy consumption is low, is suitable for industrial volume production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram (XRD) of nickel ion doped in the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope diagram (SEM) of nickel ion doped in the embodiment of the present invention 1.
Fig. 3 is the high resolution transmission electron microscopy figure (TEM) of nickel ion doped in the embodiment of the present invention 1.
Fig. 4 is the high rate performance of nickel ion doped in the embodiment of the present invention 1 and room temperature 25 DEG C and 55 DEG C of cycle performance figures of high temperature.
Detailed description of the invention
From following example it will be further appreciated that the present invention, but claimed scope is not limited to following reality
Execute the express ranges of example.
Embodiment 1
(1) manganese acetate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 5:3 adds ethanol, continue stirring and form settled solution A.
(2) ammonium hydrogen carbonate of certain mass and carbamide (ammonium hydrogen carbonate and urea quality than for 5:1) are dissolved in high purity water,
Obtain settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 2 hours at a temperature of 450 DEG C, subsequently with Quilonorm (SKB)
It is sufficiently mixed in ethanol with Nickel dichloride., is then dried under the conditions of 120 DEG C, after grinding 30 minutes, obtains presoma powder body.?
After, it is transferred to presoma powder body in high temperature furnace at 800 DEG C of hot temperature process 12 hours, cools to room temperature with the furnace and obtain nickel manganese
Acid lithium anode material.
Fig. 1 is that the X of the hollow porous nano/submicron multilevel hierarchy cubic shape nickel ion doped obtained by the present embodiment penetrates
Ray diffraction diagram is composed, the crystal structure of analysis of material.Fig. 2 is the scanning electron microscope diagram sheet of cubic shape nickel ion doped, from figure
In visible, obtained material morphology and size ratio are more uniform, are porous nano/submicron multilevel hierarchy.Fig. 3 is this enforcement
Example prepares the transmission electron micrograph of nickel ion doped particle, and obtained material presents hollow porous nano/submicron
Multilevel hierarchy.After being assembled into battery, hollow porous nano/submicron multilevel hierarchy nickel lithium manganate cathode material have excellence times
Rate performance and room temperature 25 DEG C and 55 DEG C of cycle performances of high temperature, through 100 charge and discharge cycles at room temperature 25 DEG C and high temperature 55 DEG C
Capability retention respectively up to 99.5% and 98.4%, the chemical property of these excellences come from special hollow porous nanometer/
Submicron multilevel hierarchy (see Fig. 4).
Embodiment 2
(1) manganese chloride of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 10:3 adds isopropanol, continue stirring and form settled solution A.
(2) ammonia of certain mass and carbamide (ammonia and urea quality than for 2:1) are dissolved in high purity water, are clarified
Solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 3 hours at a temperature of 500 DEG C, subsequently with hydroxide
Lithium and nickel nitrate are sufficiently mixed in ethanol, are then dried under the conditions of 120 DEG C, obtain presoma powder body after grinding 30 minutes.
Finally, it is transferred to presoma powder body in high temperature furnace at 700 DEG C of hot temperature process 15 hours, cools to room temperature with the furnace and obtain nickel
Manganate cathode material for lithium.
Embodiment 3
(1) manganese sulfate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 1:3 adds ethanol, continue stirring and form settled solution A.
(2) sodium hydroxide of certain mass is dissolved in high purity water, obtains settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 4 hours at a temperature of 400 DEG C, subsequently with lithium carbonate
It is sufficiently mixed in ethanol with nickel acetate, is then dried under the conditions of 120 DEG C, after grinding 30 minutes, obtains presoma powder body.?
After, it is transferred to presoma powder body in high temperature furnace at 650 DEG C of hot temperature process 18 hours, cools to room temperature with the furnace and obtain nickel manganese
Acid lithium anode material.
Embodiment 4
(1) manganese acetate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 2:3 adds n-butyl alcohol, continue stirring and form settled solution A.
(2) ammonium hydrogen carbonate of certain mass is dissolved in high purity water, obtains settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 2 hours at a temperature of 600 DEG C, subsequently with lithium nitrate
It is sufficiently mixed in ethanol with nickel sulfate, is then dried under the conditions of 120 DEG C, after grinding 30 minutes, obtains presoma powder body.?
After, it is transferred to presoma powder body in high temperature furnace at 900 DEG C of hot temperature process 8 hours, cools to room temperature with the furnace and obtain nickel manganese
Acid lithium anode material.
Embodiment 5
(1) manganese nitrate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 1:1 adds isobutanol, continue stirring and form settled solution A.
(2) ammonia of certain mass is dissolved in high purity water with ammonium hydrogen carbonate (ammonia and ammonium hydrogen carbonate mass ratio are 1:5),
Obtain settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 2.5 hours at a temperature of 550 DEG C, subsequently with carbonic acid
Lithium and nickel sulfate are sufficiently mixed in ethanol, are then dried under the conditions of 120 DEG C, obtain presoma powder body after grinding 30 minutes.
Finally, it is transferred to presoma powder body in high temperature furnace at 950 DEG C of hot temperature process 6 hours, cools to room temperature with the furnace and obtain nickel
Manganate cathode material for lithium.
Embodiment 6
(1) manganese nitrate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 2:1 adds normal propyl alcohol, continue stirring and form settled solution A.
(2) carbamide of certain mass is dissolved in high purity water, obtains settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 5 hours at a temperature of 400 DEG C, subsequently with lithium carbonate
It is sufficiently mixed in ethanol with Nickel dichloride., is then dried under the conditions of 120 DEG C, after grinding 30 minutes, obtains presoma powder body.?
After, it is transferred to presoma powder body in high temperature furnace at 800 DEG C of hot temperature process 10 hours, cools to room temperature with the furnace and obtain nickel manganese
Acid lithium anode material.
Embodiment 7
(1) manganese sulfate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 7:3 adds ethanol, continue stirring and form settled solution A.
(2) ammonium hydrogen carbonate of certain mass and carbamide (ammonium hydrogen carbonate and urea quality than for 1:1) are dissolved in high purity water,
Obtain settled solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 6 hours at a temperature of 350 DEG C, subsequently with hydroxide
Lithium and nickel nitrate are sufficiently mixed in ethanol, are then dried under the conditions of 120 DEG C, obtain presoma powder body after grinding 30 minutes.
Finally, it is transferred to presoma powder body in high temperature furnace at 700 DEG C of hot temperature process 14 hours, cools to room temperature with the furnace and obtain nickel
Manganate cathode material for lithium.
Embodiment 8
(1) manganese nitrate of certain mass is dissolved in the high purity water of certain volume, after fully dissolving, then according to high-purity
Water and short chain units alcohol volume ratio are that 2:3 adds ethanol, continue stirring and form settled solution A.
(2) ammonia of certain mass and carbamide (ammonia and urea quality than for 1:3) are dissolved in high purity water, are clarified
Solution B.
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation
60 minutes, after question response terminates, centrifuge washing separated and obtains nickel ion doped presoma after drying.
(4) obtained presoma is put in high temperature furnace heat treatment 4 hours at a temperature of 500 DEG C, subsequently with lithium carbonate
It is sufficiently mixed in ethanol with nickel sulfate, is then dried under the conditions of 120 DEG C, after grinding 30 minutes, obtains presoma powder body.?
After, it is transferred to presoma powder body in high temperature furnace at 750 DEG C of hot temperature process 10 hours, cools to room temperature with the furnace and obtain nickel manganese
Acid lithium anode material.
Claims (9)
1. a preparation method for anode material for lithium-ion batteries hollow porous nano/submicron multilevel hierarchy nickel ion doped, bag
Include following steps:
(1) the soluble manganese salt of certain mass is dissolved in the high purity water of certain volume, then according to high purity water and short chain units
Alcohol volume ratio is (1～10): 3 are added dropwise over short chain units alcohol, stir a period of time, obtain settled solution A；
(2) alkaline reagent of certain mass is dissolved in high purity water, obtains settled solution B；
(3) the settled solution B that step (2) prepares is joined in the settled solution A that step (1) prepares, magnetic agitation 60 points
Clock, centrifuge washing separates and obtains nickel ion doped presoma after drying；
(4) the nickel ion doped presoma that upper step obtains is put in high temperature furnace heat treatment 1～10 at a temperature of 100～1000 DEG C little
Time, it is sufficiently mixed in ethanol with lithium salts and soluble nickel salt subsequently, is then dried under the conditions of 120 DEG C, after grinding 30 minutes
Obtain presoma powder body, finally, presoma powder body is transferred in high temperature furnace heat treatment 1～20 at a temperature of 500～1000 DEG C
Hour, cool to room temperature with the furnace and obtain nickel lithium manganate cathode material.
2. preparation method as claimed in claim 1, it is characterised in that: described soluble manganese salt is manganese chloride, manganese nitrate, acetic acid
Manganese, one or more the salt-mixture in manganese sulfate.
3. preparation method as claimed in claim 1, it is characterised in that: described short chain units alcohol is ethanol, isopropanol, positive third
Alcohol, n-butyl alcohol, one or more the mixed solvent in isobutanol.
4. preparation method as claimed in claim 1, it is characterised in that: high purity water and short chain units alcohol volume ratio are (1～10):
3。
5. preparation method as claimed in claim 1, it is characterised in that: described alkaline reagent is carbamide, sodium hydroxide, ammonia,
One or more mixed base in ammonium hydrogen carbonate.
6. preparation method as claimed in claim 1, it is characterised in that: described heat treatment temperature is 100～1000 DEG C；Heat treatment
Time is 1～10 hour.
7. preparation method as claimed in claim 1, it is characterised in that: described lithium salts is Quilonorm (SKB), lithium carbonate, Lithium hydrate,
One or more mixing lithium salts of lithium nitrate.
8. preparation method as claimed in claim 1, it is characterised in that: described soluble nickel salt is: Nickel dichloride., nickel nitrate, second
Acid nickel, one or more the salt-mixture in nickel sulfate.
9. preparation method as claimed in claim 1, it is characterised in that: described heat treatment temperature is 500～1000 DEG C；Heat treatment
Time is 1～20 hour.
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