CN109301196A - A kind of method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material - Google Patents
A kind of method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material Download PDFInfo
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- CN109301196A CN109301196A CN201811086627.8A CN201811086627A CN109301196A CN 109301196 A CN109301196 A CN 109301196A CN 201811086627 A CN201811086627 A CN 201811086627A CN 109301196 A CN109301196 A CN 109301196A
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- 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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- H01M4/525—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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Abstract
The present invention relates to anode material of lithium battery technical fields, especially a kind of method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, by phosphoric acid is mixed with urea according to a certain amount of proportion, temperature reaction, not only make the phosphorus source for needing to be added secure, but also it enables to form the phosphoric acid urea structure with certain complexing function, so that by lithium source, in manganese source adition process, it is not necessary that other complexing agents are added, realize lithium source, after manganese source is added, by urea phosphate complex-precipitation, form lithium manganese phosphate ingredient, and combine the addition of nickle cobalt lithium manganate ingredient, so that nickle cobalt lithium manganate is wrapped by, not only improve the chemical property of nickel-cobalt lithium manganate cathode material, and reduce cost of material, shorten process flow.
Description
Technical field
The present invention relates to anode material of lithium battery technical field, especially a kind of lithium manganese phosphate cladding nickle cobalt lithium manganate anode
The method of material.
Background technique
With becoming increasingly conspicuous for energy and environmental problem, energy storage and conversion matchmaker of the lithium ion battery as clean and effective
One of be situated between, obtain the favor of numerous consumers.Lithium ion battery is widely used in mobile phone, laptop, camera etc.
Portable mobile apparatus.
Currently, the anode material for lithium-ion batteries of commercialization mainly has cobalt acid lithium, LiMn2O4, LiFePO4 and nickel cobalt manganese
Sour lithium etc., wherein cobalt acid lithium higher cost, when overcharge, there are security risks；Layered lithium manganate structural stability is poor, spinelle
Type LiMn2O4 specific capacity is low, and high temperature flowering structure stability is to be improved.LiFePO4 poor processability, tap density be low, energy
Density is low；In contrast, nickel-cobalt lithium manganate material is at low cost, high-temperature behavior is good, energy density is high and processing performance is excellent
The advantages that good, and then largely and widely used.But in use, it is found that the high power of nickel-cobalt lithium manganate material is forthright
Can be poor relative to cobalt acid lithium with cyclical stability, and then need to carry out its surface its chemical property of modification improvement.Currently,
Have and use carbon-coating nickel cobalt manganic acid lithium, after cladding, improves the high rate performance and cyclical stability of positive electrode.There are also uses
Fluorapatite coats nickle cobalt lithium manganate, so that cyclical stability is improved.In addition to this, there are also use manganese phosphate
Lithium coats nickel-cobalt lithium manganate cathode material, such as Patent No. 201510365733.X, reduces cost, easy popularization to reach,
And realize the purpose improved to the cyclical stability and high rate performance of nickle cobalt lithium manganate.
But it is the direction that those skilled in the art constantly pursue and research and develop for continuing to optimize for material property, and energy
It is enough so that the performance of nickel-cobalt lithium manganate cathode material is further improved and perfect, and then to nickel-cobalt lithium manganate cathode material
Improved technique further optimizes and perfect, reduction performance boost cost, enhancing chemical property become the weight of current research
Point and key technology difficulty.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of lithium manganese phosphate cladding nickel cobalt manganese
The method of sour lithium anode material.
It is achieved particular by following technical scheme:
The method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) phosphoric acid is mixed with urea according to 2:0.7-1.1, and is warming up to the mixing that 80-100 DEG C of reaction generates phosphoric acid urea
Object；After lithium carbonate, manganese nitrate are mixed according to mass ratio for 1:1, it is added to the mixture of phosphoric acid urea, is stirred evenly, is added
Enter the 20-40% that amount accounts for the mixture of phosphoric acid urea, water is added to be configured to solution, adjusting pH value is 3.8-4.1；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 60-80%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 100-120 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua
5-8h, and the drying and processing 4-5h at 50-70 DEG C, air-flow crushing cross 400 meshes；
(4) powder of step (3) is roasted into 4-5h at 600-800 DEG C, is cooled to room temperature.
It is preferred that the air-flow crushing pressure is 0.4-0.5MPa.
It is preferred that the step (3), drying temperature is 60 DEG C.
It is preferred that the step (4), maturing temperature is 700 DEG C.
It is preferred that the step (1), phosphoric acid are mixed with urea according to 2:1.
It is preferred that the manganese nitrate is replaced using manganese acetate.
Compared with prior art, the technical effect of the invention is embodied in:
By phosphoric acid is mixed with urea according to a certain amount of proportion, temperature reaction, not only to need the phosphorus source that is added
It is secure, but also enable to form the phosphoric acid urea structure with certain complexing function, so that being added by lithium source, manganese source
Cheng Zhong, without being added other complexing agents, after realizing that lithium source, manganese source are added, by urea phosphate complex-precipitation, formed lithium manganese phosphate at
Point, and the addition of nickle cobalt lithium manganate ingredient is combined to not only improve nickle cobalt lithium manganate anode material so that nickle cobalt lithium manganate is wrapped by
The chemical property of material, and cost of material is reduced, shorten process flow.
Under the invention is especially acted on through peroxophosphoric acid and urea, then cladding processing is carried out, so that the nickel prepared
The circulation chemical property of cobalt manganic acid lithium positive electrode is improved, and reduces cyclic discharge capacity attenuation rate.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
The nickel-cobalt lithium manganate material used in following embodiment is: LiNi0.5Mn0.3Co0.2O2。
Embodiment 1
The method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) phosphoric acid is mixed with urea according to 2:0.7, and is warming up to the mixture that 80 DEG C of reactions generate phosphoric acid urea；By carbonic acid
Lithium, manganese nitrate are after 1:1 is mixed, to be added to the mixture of phosphoric acid urea, stir evenly, additional amount accounts for phosphorous according to mass ratio
The 20% of the mixture of sour urea adds water to be configured to solution, and adjusting pH value is 3.8；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 60%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 100 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua 5h,
And the drying and processing 4h at 50 DEG C, under 0.4MPa pressure, air-flow crushing crosses 400 meshes；
(4) powder of step (3) is roasted into 4h at 600 DEG C, is cooled to room temperature.
Embodiment 2
The method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) phosphoric acid is mixed with urea according to 2:1.1, and is warming up to the mixture that 100 DEG C of reactions generate phosphoric acid urea；By carbonic acid
Lithium, manganese nitrate are after 1:1 is mixed, to be added to the mixture of phosphoric acid urea, stir evenly, additional amount accounts for phosphorous according to mass ratio
The 40% of the mixture of sour urea adds water to be configured to solution, and adjusting pH value is 4.1；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 80%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 120 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua 8h,
And the drying and processing 5h at 70 DEG C, under 0.5MPa pressure, air-flow crushing crosses 400 meshes；
(4) powder of step (3) is roasted into 5h at 800 DEG C, is cooled to room temperature.
Embodiment 3
The method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) phosphoric acid is mixed with urea according to 2:1, and is warming up to the mixture that 90 DEG C of reactions generate phosphoric acid urea；By lithium carbonate,
Manganese nitrate is after 1:1 is mixed, to be added to the mixture of phosphoric acid urea, stir evenly, additional amount accounts for phosphoric acid according to mass ratio
The 30% of the mixture of urea adds water to be configured to solution, and adjusting pH value is 4；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 70%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 110 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua 7h,
And the drying and processing 4.5h at 60 DEG C, under 0.45MPa pressure, air-flow crushing crosses 400 meshes；
(4) powder of step (3) is roasted into 4h at 700 DEG C, is cooled to room temperature.
Embodiment 4
The method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) phosphoric acid is mixed with urea according to 2:1.1, and is warming up to the mixture that 80 DEG C of reactions generate phosphoric acid urea；By carbonic acid
Lithium, manganese nitrate are after 1:1 is mixed, to be added to the mixture of phosphoric acid urea, stir evenly, additional amount accounts for phosphorous according to mass ratio
The 25% of the mixture of sour urea adds water to be configured to solution, and adjusting pH value is 3.9；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 80%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 100 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua 7h,
And the drying and processing 5h at 50 DEG C, under 0.5MPa pressure, air-flow crushing crosses 400 meshes；
(4) powder of step (3) is roasted into 4.5h at 800 DEG C, is cooled to room temperature.
Embodiment 5
Unlike the first embodiment, the manganese nitrate of use is that manganese acetate replaces.
Embodiment 6
Unlike the first embodiment, the manganese nitrate of use is that manganese sulfate replaces.
Embodiment 7
Unlike the first embodiment, the phosphoric acid of use is that potassium dihydrogen phosphate replaces.
As positive electrode, metal lithium sheet is negative lithium manganese phosphate cladding nickel-cobalt lithium manganate material prepared by embodiment 1-7
Pole material assembles button battery, under the voltage of 2.5-3V, and under 1C multiplying power, circulation electric discharge 200 times, and detect its appearance
Conservation rate is measured, as a result as shown in table 1 below:
Table 1
| Discharge capacity (mAh/g) for the first time | 200 discharge capacities (mAh/g) | Capacity retention ratio (%) | |
| Embodiment 1 | 172.8 | 164.5 | 4.80 |
| Embodiment 2 | 175.4 | 168.1 | 4.16 |
| Embodiment 3 | 174.6 | 167.3 | 4.18 |
| Embodiment 4 | 173.5 | 166.9 | 3.80 |
| Embodiment 5 | 178.4 | 168.7 | 5.44 |
| Embodiment 6 | 147.9 | 108.5 | 26.64 |
| Embodiment 7 | 151.6 | 109.4 | 27.84 |
| Compare (LiNi0.5Mn0.3Co0.2O2) | 150.7 | 104.8 | 30.46 |
By the data of table 1 show it can be seen from for the invention using phosphoric acid and urea effect after, then as phosphorus source
Immixture is carried out with lithium source, manganese source, and cladding after nickle cobalt lithium manganate powder is added, so that lithium manganese phosphate coats nickel cobalt mangaic acid
Lithium material effectively improves the chemical property of positive electrode, so that the stability of chemical property significantly enhances, drop
The low capacity attenuation rate of charge and discharge process.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, which comprises the following steps:
(1) phosphoric acid is mixed with urea according to 2:0.7-1.1, and is warming up to the mixing that 80-100 DEG C of reaction generates phosphoric acid urea
Object；After lithium carbonate, manganese nitrate are mixed according to mass ratio for 1:1, it is added to the mixture of phosphoric acid urea, is stirred evenly, is added
Enter the 20-40% that amount accounts for the mixture of phosphoric acid urea, water is added to be configured to solution, adjusting pH value is 3.8-4.1；
(2) solid powder nickle cobalt lithium manganate is added in the solution of step (1), additional amount is according to 60-80%(w/v)；
(3) mixed material of step (2) is stirred to evaporation at 100-120 DEG C, until solution be condensed into it is sticky after, room temperature Chen Hua
5-8h, and the drying and processing 4-5h at 50-70 DEG C, air-flow crushing cross 400 meshes；
(4) powder of step (3) is roasted into 4-5h at 600-800 DEG C, is cooled to room temperature.
2. the method for lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as described in claim 1, which is characterized in that described
Air-flow crushing pressure is 0.4-0.5MPa.
3. the method for lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as described in claim 1, which is characterized in that described
Step (3), drying temperature are 60 DEG C.
4. the method for lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as described in claim 1, which is characterized in that described
Step (4), maturing temperature are 700 DEG C.
5. the method for lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as described in claim 1, which is characterized in that described
Step (1), phosphoric acid are mixed with urea according to 2:1.
6. the method for lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as described in claim 1, which is characterized in that described
Manganese nitrate is replaced using manganese acetate.
7. the lithium manganese phosphate of as the method according to claim 1 to 6 preparation coats nickel-cobalt lithium manganate cathode material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112047321A (en) * | 2020-09-10 | 2020-12-08 | 江西智锂科技有限公司 | Method for preparing composite phosphate lithium battery anode material |
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| CN112047321A (en) * | 2020-09-10 | 2020-12-08 | 江西智锂科技有限公司 | Method for preparing composite phosphate lithium battery anode material |
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