CN109037639A - A kind of preparation method coating nickel element adulterated lithium manganate composite material - Google Patents
A kind of preparation method coating nickel element adulterated lithium manganate composite material Download PDFInfo
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- CN109037639A CN109037639A CN201810881473.5A CN201810881473A CN109037639A CN 109037639 A CN109037639 A CN 109037639A CN 201810881473 A CN201810881473 A CN 201810881473A CN 109037639 A CN109037639 A CN 109037639A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention discloses a kind of preparation methods for coating nickel element adulterated lithium manganate composite material, this method is by nine water aluminum nitrates formation solution completely soluble in water, the compound that nickel element adulterated lithium manganate obtains is added, it stirs evenly, the pH that a few drop ammonium hydroxide adjust solution are then slowly added into, after magnetic agitation 4h, are filtered, washed multiple re-dry, last 450 DEG C of calcining 3h in air atmosphere, obtain Al2O3The composite material of the nickel element adulterated lithium manganate of cladding.Present invention process is simple, at low cost, and raw material sources are extensive, is conducive to large-scale industrial production；Prepared composite material cycle performance and high rate performance are very excellent, have broad application prospects as anode material for lithium-ion batteries.
Description
Technical field
The invention belongs to technical field of new energy material preparation, are related to a kind of cladding nickel element adulterated lithium manganate composite material
Preparation method.
Background technique
As traditional fossil energy is constantly produced utilization, serious pollution is caused to environment, the mankind are to new energy
Demand it is increasing.Lithium ion battery is since high, small in size, light-weight with operating voltage, energy density is big, service life
It the advantages that long and environmentally protective, is gradually concerned by people, is the research hotspot of current new energy field.Positive electrode conduct
One of critical material of lithium ion battery is the principal element for influencing performance of lithium ion battery.However high cost and contain Co
The hypertoxicity of composite material promotes researcher to constantly look for more suitable positive electrode.Lithium manganate having spinel structure be power lithium from
Sub- battery most has one of the positive electrode of development potentiality.Therefore, lithium manganate having spinel structure is developed and utilized as lithium ion battery
Positive electrode be of great significance.
Spinel-type LiMn2O4Material is considered as with the advantages that its low cost, hypotoxicity, abundant raw material and high security
The most possible positive electrode of new generation for replacing cobalt acid lithium.However in battery use process, there is also biggish for LiMn2O4
Capacitance loss, and it is more serious under high temperature, and the cycle performance that this allows for LiMn2O4 is very poor.In order to effectively improve LiMn2O4
Cycle performance and high rate performance, bulk phase-doped and surface modification become improved main path.Bulk phase-doped is from intracell
Improve one of the effective ways of lithium manganate having spinel structure positive electrode chemical property.It is mentioned by adulterating some metal cations
The average valence of high Mn ion, prevents the generation of battery Jahn-Teller effect in charge and discharge process, to make the knot of positive electrode
Structure stability greatly improves.The change of material structure caused by the dissolution of Mn is also to influence to improve LiMn2O4Chemical property
One factor partially replaces Mn by adulterating other metal ions to this3+The dissolution of Mn is just effectively prevented, and then is improved
Chemical property.Surface coating modification is to inhibit the dissolution of Mn and and prevent electrolyte from decomposing and then improving on the electrode
LiMn2O4A kind of effective ways of chemical property under high-temperature can be classified as organic according to the difference of covering material
Object surface cladding and inorganic, metal oxide surface cladding.Jinhua Cao et al. prepares carbon packet using high-temperature solid combustion method
Cover LiMn2O4Composite material, though by electrochemical behavior test display initial discharge capacity it is higher, reach 132mAh/g, its
It reacts more demanding, (Jinhua Cao et al.Carbon-coated single- need to be reacted under 750 DEG C of high temperature
crystalline LiMn2O4 nanowires synthesized by high-temperature solid-state
reaction with high capacity for Li-ion battery[J].Journal of Alloys and
Compounds,2018).Qi-Ling Li et al. people prepares ZnO cladding LiMn using combustion method2O4Composite material, in contrast to
The pure phase LiMn2O4 of cladding, though having preferable cyclical stability, first discharge specific capacity is only in 118mAh/g or so (Qi-
Ling Li et al.ZnO-coated LiMn2O4 cathode material for lithium-ion batteries
Synthesized by a combustion method [J] .Ionics, 2016).
Summary of the invention
The object of the present invention is to provide a kind of preparation methods for coating nickel element adulterated lithium manganate composite material.
Realizing the technical solution of the object of the invention is:
A kind of preparation method coating nickel element adulterated lithium manganate composite material, the specific steps are as follows:
Step 1, manganese carbonate, nickel acetate tetrahydrate, lithium carbonate are weighed in molar ratio for 1.5:0.5:2, a few drop nothings is added
80 DEG C of dry 12h after water-ethanol is fully ground, are placed in Muffle furnace, grind after the lower 450 DEG C of pre-burnings of air atmosphere, 750 DEG C of high temperature
Lower calcining 18h obtains the composite L iNi of nickel element adulterated lithium manganate0.5Mn1.5O4；
Step 2, nine water aluminum nitrates are stirred to soluble in water, formation homogeneous solution.Again by the nickel prepared in step 1 member
The compound LiNi that plain adulterated lithium manganate obtains0.5Mn1.5O4It is added in aluminum nitrate solution, is uniformly mixed, ammonium hydroxide is added dropwise
After adjusting pH to 9 ± 1, magnetic agitation 4h, it is filtered, washed re-dry and obtains presoma；
Step 3, by presoma 450 ± 50 DEG C of calcinings in air atmosphere, Al is obtained2O3The nickel element of cladding adulterates mangaic acid
The composite A l of lithium2O3/LiNi0.5Mn1.5O4。
Preferably, in step 2, the pH is 9.
Preferably, in step 2, the washing is distillation water washing 3 times, and dehydrated alcohol washs 3 times.
Preferably, in step 3, the presoma calcination temperature is 450 DEG C.
Preferably, in step 3, heating rate is 5 DEG C/min.
Compared with prior art, the invention has the following advantages that
(1) Al of the method for the present invention preparation2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/
LiNi0.5Mn1.5O4, Al2O3Preferably reduce contact of the positive electrode with electrolyte as clad, thus reduce manganese from
The dissolution of son, improves cycle performance, high rate performance and safety；
(2) Al of the method for the present invention preparation2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/
LiNi0.5Mn1.5O4, a small amount of Al2O3Cladding is to LiMn2O4The crystal structure of material does not have an impact, because of Al2O3With good
Highly electron conductive possessed by chemical stability and amphoteric oxide makes the positive electrode chemical property of preparation obtain pole
Big improvement.
Detailed description of the invention
Fig. 1 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4XRD diagram.
Fig. 2 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4(a) and nickel element
The composite L iNi of adulterated lithium manganate0.5Mn1.5O4(b) TEM partial enlarged view.
Fig. 3 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4Cycle performance curve graph.
Fig. 4 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4The high rate performance figure under different current densities.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1
(1) preparation of aluminum nitrate solution: when preparing solution, weighing nine water aluminum nitrates and be dissolved in 40ml deionized water, stirs
Until being completely dissolved；
(2) the compound LiNi that nickel element adulterated lithium manganate obtains0.5Mn1.5O4Preparation: will by manganese carbonate, four hydration second
Sour nickel, lithium carbonate weigh in molar ratio for 1.5:0.5:2, and 80 DEG C of dry 12h after a few drop dehydrated alcohols are fully ground are added, are placed in
It in Muffle furnace, is ground after the lower 450 DEG C of pre-burnings of air atmosphere, 18h is calcined under 750 DEG C of high temperature and obtains answering for nickel element adulterated lithium manganate
Condensation material LiNi0.5Mn1.5O4；
(3) preparation of mixed liquor: the compound LiNi that nickel element adulterated lithium manganate is obtained0.5Mn1.5O4Powder is added to
(1) in solution, magnetic agitation is formed uniformly mixed liquor；
(4) it the preparation of presoma: after the pH to 9 of dropwise addition ammonium hydroxide adjusting mixed liquor (3), magnetic agitation 4h, is filtered, washed again
It is dried to obtain presoma；
(5) calcining of presoma: by above-mentioned presoma in air atmosphere 450 DEG C of calcining 3h to get Al2O3The nickel of cladding
The composite A l of element doping LiMn2O42O3/LiNi0.5Mn1.5O4。
Fig. 1 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4XRD diagram, it is known that each diffraction maximum of covering material with nickel element adulterate mangaic acid
The composite L iNi of lithium0.5Mn1.5O4Diffraction maximum is almost the same, and free from admixture peak, belongs to spinel structure and Fd3m space group,
This, which also shows, uses Al2O3To LiNi0.5Mn1.5O4Particle carries out surface cladding without changing LiNi0.5Mn1.5O4Lattice structure.
Fig. 2 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4(a) and nickel element
The composite L iNi of adulterated lithium manganate0.5Mn1.5O4(b) TEM partial enlarged view, as seen from the figure Al2O3Preferable cladding
In the composite L iNi of nickel element adulterated lithium manganate0.5Mn1.5O4Particle surface, surface coated Al2O3It can reduce
LiNi0.5Mn1.5O4With the contact area of electrolyte, therefore Mn can be inhibited to a certain extent3+Dissolution, and then improve its electricity
Chemical property.
Fig. 3 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4Cycle performance curve graph.As shown in figure 3, Al2O3The nickel element of cladding adulterates
The composite A l of LiMn2O42O3/LiNi0.5Mn1.5O4With preferable cyclical stability, first discharge specific capacity 127mAh/
G, capacity retention ratio is up to 92% after recycling 50 times.In contrast, the composite material of uncoated nickel element adulterated lithium manganate
LiNi0.5Mn1.5O4Though the more a height of 130mAh/g of first discharge specific capacity, capacity attenuation is very fast, and capacity retention ratio only reaches
87%, mainly as caused by the dissolution of manganese ion and electrolyte.Therefore, Al2O3Coat LiNi0.5Mn1.5O4Preferably improve material
The structural stability of material, to improve its chemical property.
Fig. 4 is Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is mixed with nickel element
The composite L iNi of miscellaneous LiMn2O40.5Mn1.5O4The high rate performance figure under different current densities.Selection 0.1C, 0.2C,
The current density of 0.5C, 1.0C, 2.0C carry out high rate performance test, and electric current is gradually increased in test process, by the big of 2.0C
After electric current, it is gradually reduced electric current, is restored to initial low current, sees the recovery of its capacity, investigates the high rate performance of material.
Each current density loop test 10 times, it is as shown in Figure 4 to obtain result.As seen from the figure, with the increase of current density, specific capacity
Reducing, and Al2O3The composite A l of the nickel element adulterated lithium manganate of cladding2O3/LiNi0.5Mn1.5O4It is close in different electric currents
Capacity retention ratio is all higher than the composite L iNi of nickel element adulterated lithium manganate when circulation under degree0.5Mn1.5O4, extensive in current density
Specific capacity does not almost reduce when arriving 0.1C again, shows excellent multiplying power property.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, unique the difference is that using ammonium hydroxide in the preparation process of (3) presoma
The pH for adjusting mixed liquor is respectively 8,10, the chemical property of resulting materials almost indifference when with the pH of solution being 9, solution
Resulting materials have better crystallinity when pH is 9.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, unique the difference is that calcining is warm in the calcination process of (4) presoma
Degree is 400 DEG C, 500 DEG C, is 450 DEG C of sample chemical properties prepared almost indifference with calcination temperature, after recycling 50 times
Capacity retention ratio can reach 92% or so.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that using 650 in the calcination process of (4) presoma
It is calcined at DEG C, calcination temperature is higher to result in intergranular serious agglomeration, and the material prepared either cycle performance is also
Be high rate performance it is bad and 650 DEG C under conditions of energy loss it is larger.
Comparative example 2
Al2O3The composite L iNi of nickel element adulterated lithium manganate is significantly improved as clad0.5Mn1.5O4Electricity
Chemical property.Change Al2O3Covering amount to LiNi0.5Mn1.5O4It is coated to obtain composite material 1wt%Al2O3/
LiNi0.5Mn1.5O4, 3wt%Al2O3/LiNi0.5Mn1.5O4, 5wt%Al2O3/LiNi0.5Mn1.5O4, carry out electrochemical property test
It was found that capacity retention ratio is respectively 86%, 92%, 87%, therefore, with mass fraction after with 0.1C current density circulation 50 times
For 3% Al2O3As clad to the composite L iNi of nickel element adulterated lithium manganate0.5Mn1.5O4Carry out covered effect most
Good, chemical property is optimal.
Claims (4)
1. a kind of preparation method for coating nickel element adulterated lithium manganate composite material, which is characterized in that specific step is as follows:
Step 1, manganese carbonate, nickel acetate tetrahydrate, lithium carbonate are weighed in molar ratio for 1.5:0.5:2, a few anhydrous second of drop is added
80 DEG C of dry 12h after alcohol is fully ground, are placed in Muffle furnace, grind after the lower 450 DEG C of pre-burnings of air atmosphere, forge under 750 DEG C of high temperature
It burns 18h and obtains the composite L iNi of nickel element adulterated lithium manganate0.5Mn1.5O4；
Step 2, nine water aluminum nitrates are dissolved in deionized water and form solution, the nickel element adulterated lithium manganate prepared is added and obtains
The compound LiNi arrived0.5Mn1.5O4, stir evenly to form mixed solution；It is then slowly added into ammonium hydroxide and adjusts solution PH to 9 ± 1,
After magnetic agitation 4h, it is filtered, washed multiple re-dry, obtains presoma；
Step 3, by presoma 450 ± 50 DEG C of calcinings in air atmosphere, Al is obtained2O3The nickel element adulterated lithium manganate of cladding
Composite A l2O3/LiNi0.5Mn1.5O4。
2. the preparation method of cladding nickel element adulterated lithium manganate composite material according to claim 1, which is characterized in that step
In rapid 2, the PH that ammonium hydroxide adjusts solution is 9.
3. the preparation method of cladding nickel element adulterated lithium manganate composite material according to claim 1, which is characterized in that step
In rapid 3, calcination temperature is 450 DEG C, and calcination time is 3~5h.
4. the preparation method of cladding nickel element adulterated lithium manganate composite material according to claim 1, which is characterized in that step
In rapid 3, heating rate is 3~5 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110311101A (en) * | 2019-06-12 | 2019-10-08 | 常州大学 | Li1.2Ni0.13Co0.13Mn0.54O2/Al2O3The preparation method of composite material |
| CN110773112A (en) * | 2019-09-25 | 2020-02-11 | 中国科学院青海盐湖研究所 | Modified manganese-based lithium ion sieve and preparation method thereof |
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| CN110773112A (en) * | 2019-09-25 | 2020-02-11 | 中国科学院青海盐湖研究所 | Modified manganese-based lithium ion sieve and preparation method thereof |
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Application publication date: 20181218 |