CN110190276A - A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries - Google Patents
A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries Download PDFInfo
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- CN110190276A CN110190276A CN201910621310.8A CN201910621310A CN110190276A CN 110190276 A CN110190276 A CN 110190276A CN 201910621310 A CN201910621310 A CN 201910621310A CN 110190276 A CN110190276 A CN 110190276A
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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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- 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 invention discloses the preparation methods of a kind of niobium, aluminium codope anode material for lithium-ion batteries, by nickel manganese hydroxide precursor Ni0.75Mn0.25(OH)2And Li2CO3It is scattered in formation suspension A in dehydrated alcohol；By LiNbO3And Al2O3It is scattered in formation suspension B in dehydrated alcohol；Suspension A and suspension B is mixed to be placed in water-bath and stirs into mixture of viscous form material, drying in air dry oven is transferred to and obtains presoma；Presoma is transferred in atmosphere furnace, 400 ~ 600 DEG C of 5 ~ 10h of pretreatment are warming up to the heating rate of 1 ~ 5 DEG C/min in air atmosphere, then is warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtains the lithium-rich anode material of niobium, aluminium codope.Anode material for lithium-ion batteries produced by the present invention can effectively inhibit the problem that material voltage attenuation is very fast in cyclic process, and be effectively improved the stable circulation performance of positive electrode and improve the specific discharge capacity of positive electrode.
Description
Technical field
The invention belongs to the preparation technical fields of lithium-enriched cathodic material of lithium ion battery, and in particular to a kind of niobium, aluminium are co-doped with
The preparation method of miscellaneous anode material for lithium-ion batteries.
Background technique
The energy is that human society is rely the foundation stone of development.Since the industrial revolution, conventional fossil fuel is the hair of human society
Exhibition is made that indelible contribution, but its additional the problems such as bringing chemical fumes, Particulate Pollution.The sustainable of the energy opens
Adopting application is the challenge that countries in the world today will must face and receive.It is brought with the exhaustion and its of fossil energy resource
Environmental problem, developing green clean energy resource becomes the hot spot that the whole world is paid close attention to and studied.Solar energy, wind energy, ocean energy etc. are each
Kind green energy resource naturally has fluctuation intermittence etc., how to store and efficiently use on a large scale these new energy, energy storage skill
Art-lithium ion secondary battery is exactly the important medium of energy conversion among these.
The 1990s LiCoO2Realize that commercialization is used, but Co valence persistently rises, enterprise's production cost increases, and Co
For heavy metal, there is pollution to environment.LiNi1-x-yCoxMnyO2/LiNi1-x-yCoxAlyO2Equal ternary materials are with respect to cobalt acid lithium specific volume
Measure higher, cost decline.But the stability of lower efficiency for charge-discharge, material structure, poor high rate performance etc. still need
Further research is modified.Electric car is popularized, and extensive use of smart grid etc. requires higher and higher get over to lithium ion battery
Come more clear, i.e. high-energy density, high power, high circulation service life, environmental protection, cost etc..Stratiform richness lithium manganese oxide becomes industry
New focusing research hotspot.Its synthesis technology is simple first, and material, subsequent heat treatment sintering can be mass produced in coprecipitation
Technique does not need inert atmosphere protection.Material component is environmental-friendly without Co lower production costs, and discharge capacity is higher, in electric discharge
Threshold voltage and more mature electrolyte fitness in the market are higher.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple process and low-cost niobiums, aluminium codope lithium ion
The preparation method of cell positive material, anode material for lithium-ion batteries made from this method can effectively inhibit material in cyclic process
Expect the very fast problem of voltage attenuation, and is effectively improved the stable circulation performance of positive electrode and improves the electric discharge specific volume of positive electrode
Amount.
The present invention adopts the following technical scheme that solve above-mentioned technical problem
A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3
Be sequentially placed into reaction vessel and be added the quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；
Step S2: by the LiNbO of 0.01 ~ 0.05 parts by weight3With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel
And dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of pretreatment, then be warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtain the lithium-rich anode material of niobium, aluminium codope.
A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3
Be sequentially placed into reaction vessel and be added the quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；
Step S2: by the Nb of 0.01 ~ 0.03 parts by weight2O5With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel
And dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of pretreatment, then be warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtain the lithium-rich anode material of niobium, aluminium codope.
A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is placed in reaction vessel
And be added the quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；
Step S2: by the LiNbO of 0.01 ~ 0.05 parts by weight3With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel
And dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of processing obtain the lithium-rich anode material of niobium, aluminium codope.
A kind of preparation method of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is placed in reaction vessel
And dehydrated alcohol is added and is quickly uniformly mixed to form suspension A；
Step S2: by the Li of 0.01 ~ 0.03 parts by weight2CO3, 0.01 ~ 0.03 parts by weight Nb2O5With 0.01 ~ 0.05 parts by weight
Al2O3It is sequentially placed into reaction vessel and dehydrated alcohol ultrasonic disperse is added and be formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of processing obtain the lithium-rich anode material of niobium, aluminium codope.
Preferably, the LiNbO3For commercialized LiNbO3, the LiNbO3It is first placed in ball grinder and refines before the use
Grain diameter.
Compared with the prior art, the invention has the following beneficial effects: synthesis technology of the present invention is simple, using coprecipitation
It can be realized the large-scale production of anode material for lithium-ion batteries, anode material for lithium-ion batteries produced by the present invention can be effective
Inhibit the problem that material voltage attenuation is very fast in cyclic process, and is effectively improved the stable circulation performance of positive electrode and improves just
The specific discharge capacity of pole material.
Detailed description of the invention
Fig. 1 is the embodiment of the present invention 2 and comparative example 1 obtains the first charge-discharge song that lithium ion battery is made in positive electrode
Line；
Fig. 2 is the embodiment of the present invention 2 and comparative example 1 obtains the charge and discharge song that 100 circle of lithium ion battery circulation is made in positive electrode
Line；
Fig. 3 is that the embodiment of the present invention 2 and comparative example 1 obtain cycle performance of lithium ion battery curve made from positive electrode.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
By the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3Successively put
Enter in beaker, be added the quick magnetic agitation of a certain amount of dehydrated alcohol be uniformly mixed obtain suspension A；By 0.01 ~ 0.05 weight
The LiNbO of part3With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into beaker, a certain amount of dehydrated alcohol ultrasonic disperse is added
It is formed uniformly suspension B, the LiNbO3For commercialized LiNbO3, the LiNbO3It is first placed in ball grinder before the use thin
Change grain diameter；Then suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick
Mixed material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；Finally presoma is shifted
Into atmosphere furnace, 400 ~ 600 DEG C of 5 ~ 10h of pretreatment are warming up to the heating rate of 1 ~ 5 DEG C/min in air atmosphere, then heat up
The lithium-rich anode material of Nb, Al codope is obtained to 700 ~ 900 DEG C of 10 ~ 15h of sintering.
Embodiment 2
By the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3Successively put
Enter in beaker, be added the quick magnetic agitation of a certain amount of dehydrated alcohol be uniformly mixed form suspension A；By 0.01 ~ 0.03 weight
The Nb of part2O5With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into beaker, it is equal that a certain amount of dehydrated alcohol ultrasonic disperse is added
Even formation suspension B；Then suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at sticky
Shape mixed material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；Finally presoma is turned
It moves in atmosphere furnace, 400 ~ 600 DEG C of 5 ~ 10h of pretreatment is warming up to the heating rate of 1 ~ 5 DEG C/min in air atmosphere, then rise
Temperature obtains the lithium-rich anode material of Nb, Al codope to 700 ~ 900 DEG C of 10 ~ 15h of sintering.
Embodiment 3
By the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is put into beaker, is added a certain amount of
The quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；By the LiNbO of 0.01 ~ 0.05 parts by weight3With 0.01 ~
The Al of 0.05 parts by weight2O3It is sequentially placed into beaker, a certain amount of dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B, institute
State LiNbO3For commercialized LiNbO3, the LiNbO3It is first placed in micronized particles partial size in ball grinder before the use；Then it will hang
Turbid A and suspension B mixing is placed in water-bath, and the quick magnetic agitation of constant temperature, then will be thick at mixture of viscous form material
Mixed material is transferred to drying in air dry oven and obtains presoma；Finally presoma is transferred in atmosphere furnace, in air gas
400 ~ 600 DEG C of 5 ~ 10h of processing are warming up to the heating rate of 1 ~ 5 DEG C/min under atmosphere and obtain the lithium-rich anode material of Nb, Al codope
Material.
Embodiment 4
By the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is put into beaker, is added a certain amount of
The quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；By the Li of 0.01 ~ 0.03 parts by weight2CO3、0.01~0.03
The Nb of parts by weight2O5With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into beaker, a certain amount of dehydrated alcohol ultrasound point is added
It dissipates and is formed uniformly suspension B；Then suspension A and suspension B are mixed and are placed in water-bath, the quick magnetic agitation of constant temperature at
Mixture of viscous form material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；Finally by forerunner
Body is transferred in atmosphere furnace, is warming up to 400 ~ 600 DEG C of 5 ~ 10h of processing in air atmosphere with the heating rate of 1 ~ 5 DEG C/min and is obtained
To the lithium-rich anode material of Nb, Al codope.
Comparative example 1
By the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3Successively put
Enter in beaker, be added the quick magnetic agitation of a certain amount of dehydrated alcohol be uniformly mixed form suspension；Suspension is placed in water-bath
In pot, the quick magnetic agitation of constant temperature is at mixture of viscous form material, then mixture of viscous form material is transferred in air dry oven and is dried
It is dry to obtain presoma；Finally presoma is transferred in atmosphere furnace, is heated up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min
To 400 ~ 600 DEG C of 5 ~ 10h of pretreatment, then it is warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtains the Ni, Mn oxide anode material of rich lithium
Material.
Half-cell is prepared using positive electrode made from embodiment and comparative example.Cycle performance is tested in charge-discharge magnification
To carry out (wherein first three circle carries out material activation using 0.1C current density) under conditions of 1C.Charging/discharging voltage range: 2.1-
4.8V；Measurement result is shown in Table 1.The first charge-discharge curve that lithium ion battery is made in different samples is shown in Fig. 1,100 recyclings
Lithium ion battery charging and discharging curve afterwards is shown in that Fig. 2, the cycle performance curve of lithium ion battery are shown in Fig. 2.
The cycle performance test result of lithium ion battery made from the different samples of table 1
| Sample number into spectrum | Coulombic efficiency (%) for the first time | First discharge specific capacity (mAh/g) | 4 specific discharge capacities (mAh/g) | 50 specific discharge capacities (mAh/g) | 100 specific discharge capacities (mAh/g) | Capacity retention ratio (%) under 1C current density |
| Embodiment 1 | 73.57 | 241.8 | 176.2 | 170.1 | 165.9 | 94.15 |
| Embodiment 2 | 74.59 | 247.6 | 177.8 | 173.8 | 170.2 | 95.73 |
| Embodiment 3 | 70.3 | 243.2 | 177.1 | 169.3 | 163.8 | 92.49 |
| Embodiment 4 | 70.13 | 248.3 | 174.9 | 169.5 | 162.2 | 92.74 |
| Comparative example 1 | 65.88 | 242.4 | 172.2 | 161.3 | 157.3 | 91.35 |
Embodiment above describes basic principles and main features of the invention and advantages, It should be understood by those skilled in the art that
The present invention is not limited to the above embodiments, and the above embodiments and description only illustrate the principle of the present invention,
Under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements each fall within this hair
In the range of bright protection.
Claims (5)
1. the preparation method of a kind of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3
Be sequentially placed into reaction vessel and be added the quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；
Step S2: by the LiNbO of 0.01 ~ 0.05 parts by weight3With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel
And dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of pretreatment, then be warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtain the lithium-rich anode material of niobium, aluminium codope.
2. the preparation method of a kind of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the nickel manganese hydroxide precursor Ni of 2 ~ 3 parts by weight0.75Mn0.25(OH)2With the Li of 0.5 ~ 2 parts by weight2CO3
Be sequentially placed into reaction vessel and be added the quick magnetic agitation of dehydrated alcohol be uniformly mixed form suspension A；
Step S2: by the Nb of 0.01 ~ 0.03 parts by weight2O5With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel simultaneously
Dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of pretreatment, then be warming up to 700 ~ 900 DEG C of 10 ~ 15h of sintering and obtain the lithium-rich anode material of niobium, aluminium codope.
3. the preparation method of a kind of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is placed in reaction vessel simultaneously
The addition quick magnetic agitation of dehydrated alcohol, which is uniformly mixed, forms suspension A；
Step S2: by the LiNbO of 0.01 ~ 0.05 parts by weight3With the Al of 0.01 ~ 0.05 parts by weight2O3It is sequentially placed into reaction vessel
And dehydrated alcohol ultrasonic disperse is added and is formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of processing obtain the lithium-rich anode material of niobium, aluminium codope.
4. the preparation method of a kind of niobium, aluminium codope anode material for lithium-ion batteries, it is characterised in that specific steps are as follows:
Step S1: by the rich Li, Ni, Mn oxide positive electrode Li of 1 ~ 3 parts by weight1.2(Mn0.6Ni0.2)O2It is placed in reaction vessel simultaneously
Dehydrated alcohol is added quickly to be uniformly mixed to form suspension A；
Step S2: by the Li of 0.01 ~ 0.03 parts by weight2CO3, 0.01 ~ 0.03 parts by weight Nb2O5With 0.01 ~ 0.05 parts by weight
Al2O3It is sequentially placed into reaction vessel and dehydrated alcohol ultrasonic disperse is added and be formed uniformly suspension B；
Step S3: suspension A and suspension B is mixed and is placed in water-bath, the quick magnetic agitation of constant temperature is at thick mixing
Material, then mixture of viscous form material is transferred to drying in air dry oven and obtains presoma；
Step S4: presoma is transferred in atmosphere furnace, 400 are warming up in air atmosphere with the heating rate of 1 ~ 5 DEG C/min ~
600 DEG C of 5 ~ 10h of processing obtain the lithium-rich anode material of niobium, aluminium codope.
5. the preparation method of niobium according to claim 1 or 3, aluminium codope anode material for lithium-ion batteries, feature exist
In: the LiNbO3For commercialized LiNbO3, the LiNbO3It is first placed in micronized particles partial size in ball grinder before the use.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102694165A (en) * | 2012-06-08 | 2012-09-26 | 天津理工大学 | High-capacity lithium-rich layered crystalline structured lithium battery cathode material and preparation thereof |
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