CN108493435A - Anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2And preparation method - Google Patents
Anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2And preparation method Download PDFInfo
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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Abstract
The invention belongs to field of lithium ion battery, provide anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1‑xYxO2And preparation method thereof, wherein 0<X≤0.05, to overcome LiNi0.8Mn0.1Co0.1O2Electrochemistry poor circulation and the bad disadvantage of security performance.The present invention is reduced the cationic mixing of material by the doping of minimal amount of yttrium, is expanded Li using bulk phase-doped modified+Diffusion admittance improves Li in material+Diffusivity, stabilize the internal structure of material, considerably enhance the cyclical stability of material；And have the function of storing up oxygen using metal ruthenium ion, when large scale takes off lithium to material under high voltages, Ni in material4+Ion has high oxidation activity, and ruthenium ion has absorption O2‑Function, Ni can be made4+Ion surface is passivated, and is weakened to the oxidisability of electrolyte, to improve the safety of charge and discharge under high voltage；The LiYO of Surface Creation simultaneously2Lithium fast-ionic conductor not only increases ionic conductivity, and the surface alkalinty of material is made to decline.Anode material for lithium-ion batteries i.e. of the present invention disclosure satisfy that compared with high rate charge-discharge and high-energy density demand, and greatly improve the safety under the conditions of its high voltage charge and discharge.
Description
Technical field
The invention belongs to field of lithium ion battery, are related to anode material for lithium-ion batteries and preparation method thereof, specially lithium
Ion battery positive electrode Li (Ni0.8Co0.1Mn0.1)1-xYxO2And preparation method thereof, wherein 0<x≤0.05.
Background technology
Under new energy materials research and development and the promotion of related industry, anode material for lithium-ion batteries is just close towards higher energy
Degree, energy density per unit volume, cycle life, safety and the direction fast development of lower cost.In miscellaneous positive material
Industrialized positive electrode is mainly the following at present in material：Cobalt acid lithium, LiFePO4, LiMn2O4 and ternary material；
Wherein ternary material according to chemical composition can be divided into nickel cobalt manganese and nickel cobalt aluminium two major classes again.Nickelic nickel-cobalt-manganese ternary anode material
Material be different from the lower tertiary cathode material of traditional nickel content (111 types, 424 types, 523 types) its nickel content be higher than 0.6, it is nickelic
Tertiary cathode material has many advantages, such as that energy density is high, at low cost, is becoming industrialization power lithium-ion battery in recent years just
The hot spot researched and developed and produced in the material of pole.
However, nickelic tertiary cathode material is as nickel content is when being stepped up, wherein Ni2+And Li+Cation it is mixed
Arranging phenomenon will be even more serious, and the cyclical stability so as to cause material is not highly desirable；In order to improve nickelic tertiary cathode
The bad problem of cyclical stability in material can usually use the modified methods such as doping, cladding.Relative to cladding, the work of doping
Skill is more simple, it is easier to and it realizes industrialization, but adulterates the element with electro-chemical activity that often substitution is a small amount of, to
Reduce the specific discharge capacity of material.
Invention content
It is an object of the invention to be directed to the nickelic nickle cobalt lithium manganate of anode material for lithium-ion batteries stratiform
(LiNi0.8Mn0.1Co0.1O2) electrochemistry poor circulation and the bad disadvantage of security performance, a kind of lithium excess combination phase is provided
Anode material for lithium-ion batteries Li (the Ni of doping vario-property0.8Co0.1Mn0.1)1-xYxO2And preparation method thereof, wherein 0<x≤0.05.
Anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2With very high specific discharge capacity and excellent stable circulation
Performance disclosure satisfy that compared with high rate charge-discharge demand, and improve the safety under the conditions of its high voltage charge and discharge, prepare
Method carries out bulk phase-doped, operating process and simple for process using traditional solid phase method, it is easy to accomplish industrialized production, product knot
Brilliant quality is high, particle is tiny, be evenly distributed and manufacturing cost is low.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2, which is characterized in that the lithium ion battery
The biomolecule expressions of positive electrode are Li (Ni0.8Co0.1Mn0.1)1-xYxO2, wherein 0<x≤0.05.
Above-mentioned anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2Preparation method, which is characterized in that including
Following steps：
Lithium source dissolution of raw material in deionized water, is added yttrium and expects to be uniformly mixed in a steady stream, grinding obtains mixing slurry by step 1.
Material, wherein molar ratio Li：Y=(1.1~1.2)：x、0<x≤0.05；
Ni is added in gained mixed slurry in step 1 by step 2. wherein0.8Co0.1Mn0.1(OH)2Presoma and anhydrous second
Alcohol continues to grind, until mixed slurry is abnormal in uniform flow, then continues to be ground under infrared lamp and goes completely into mixed-powder,
Wherein, molar ratio Li：Ni0.8Co0.1Mn0.1(OH)2：Y=(1.1~1.2)：1-x：x；
Mixed-powder after grinding uniformly obtained by step 2 is placed in tube furnace under oxygen atmosphere first with 2 by step 3.
~5 DEG C/min is warming up to 470~550 DEG C of 6~10h of pre-burning, then with 2~3 DEG C/min be warming up to 750~850 DEG C of roastings 15~
20h, then 450~500 DEG C are cooled to 2 DEG C/min programs, it finally cools to room temperature with the furnace, obtains Li
(Ni0.8Co0.1Mn0.1)1-xYxO2。
In step 1 and step 2, the molar ratio of the lithium source raw material, yttrium source raw material and presoma be (1.10~
1.20):x:(1-x)。
In step 1, the lithium source raw material be lithium carbonate, lithium nitrate, lithium acetate, lithium chloride and lithium hydroxide at least
It is a kind of.
In step 1, yttrium source raw material be yttrium nitrate, yttrium hydroxide, yttrium sulfate, yttrium chloride and yttrium oxide in
It is at least one.
From operation principle：The present invention is in nickelic tertiary cathode material LiNi0.8Mn0.1Co0.1O2In be doped with it is a small amount of
Metallic element yttrium, the metallic element yttrium of trivalent can rely on its larger ionic radius (0.090nm) that material unit cell volume is made to increase
Greatly, to expand Li+Abjection and embedded path, reduce Li+The resistance of deintercalation, while also reducing Li+Deintercalation process is to crystal
Structural damage stabilizes the skeleton structure of material, improves the chemical property of material, also improves material crystal structure
Stability；Meanwhile inside metallic element ruthenium ion incorporation material lattice, material granule can be made to refine and evenly, increase material
The electric conductivity of material；In addition, the addition of excessive lithium source can overcome the disadvantages that the lithium loss of material at high temperature, make to have in material more
Lithium ion further increases the energy density of material to possess higher specific discharge capacity.What is more important, due to gold
Belonging to ruthenium ion has the function of oxygen overflow and storage oxygen, when large scale takes off lithium to material under 4.5V high voltages, Ni in material4+Ion
Ratio improves, a large amount of Ni4+Ion has high oxidation activity, and ruthenium ion has absorption O2-Function, Ni can be made4+From
Sublist face occurs passivation and (is reduced to stable Ni3+), thus the oxidisability of electrolyte is weakened, it is filled under high voltage to improve
The safety of electric discharge.It has also been found that due to the addition of Y, the LiYO after thickness is about 5-20nm is generated in material surface2
Lithium fast-ionic conductor not only increases ionic conductivity, and the surface alkalinty of material is made to decline, and pH value reduces, cost performance
It is obviously improved.
In conclusion the invention has the advantages that：
1, the present invention reduces the cationic mixing of material by the doping of minimal amount of yttrium, expands Li+Diffusion is logical
Road improves Li in material+Diffusivity, stabilize the internal structure of material, considerably enhance material high rate performance and
Cyclical stability.
2, layered lithium ion battery positive electrode Li (Ni prepared by the present invention0.8Co0.1Mn0.1)1-xYxO2, pass through larger lithium
Excessive 10%~20%, the lithium loss of material at high temperature is compensated for, the specific discharge capacity of material is increased.
3, present invention utilizes metal ruthenium ions to have the function of storing up oxygen (high-temperature fuel cell is often with this function), works as material
When large scale takes off lithium under high voltages, Ni in material4+Ion has high oxidation activity, and ruthenium ion has absorption O2-'s
Function can make Ni4+Ion surface is passivated, and is weakened to the oxidisability of electrolyte, to improve charge and discharge under high voltage
Safety.
4, layered lithium ion battery positive electrode Li (Ni prepared by the present invention0.8Co0.1Mn0.1)1-xYxO2With high electric discharge
Specific capacity and very excellent cycle performance；Under room temperature environment, when voltage range is in 2.8~4.3V, constant current charge-discharge times
When rate is 0.5C, the first discharge specific capacity of the anode material for lithium-ion batteries can reach 180.4mAh g-1, cycle 100 times with
It still can reach 183.9mAh g afterwards-1, capacity retention ratio is up to 101.9%；When voltage range is in 2.8~4.5V, constant current charge and discharge
When electric multiplying power is 0.5C, the initial discharge specific capacity of the anode material for lithium-ion batteries can reach 192.0mAh g-1, cycle 100
189.4mAh g are still can reach after secondary-1, capacity retention ratio 98.6%.
5, the present invention generates the LiYO after thickness is about 5-20nm due to the addition of Y in material surface2The fast ion of lithium is led
Body not only increases ionic conductivity, and the surface alkalinty of material is made to decline, and pH value reduces, and processing performance has obtained obviously
Improve.
6, technological process of the invention is simple and environmentally protective, and device therefor is also relatively simple in technique, and raw material sources are extensive,
It is easily achieved large-scale industrial production.
Description of the drawings
Fig. 1 is that the present invention prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2Process flow chart.
Fig. 2 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2XRD diagram.
Fig. 3 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2SEM figure.
Fig. 4 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO22.8~
In 4.3V voltage ranges, with 0.5C rate charge-discharges, initial charge/discharge curve graph.
Fig. 5 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO22.8~
In 4.3V voltage ranges, with 0.5C rate charge-discharges, cycle performance curve graph.
Fig. 6 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO22.8~
In 4.5V voltage ranges, with 0.5C rate charge-discharges, initial charge/discharge curve graph.
Fig. 7 is that the embodiment of the present invention 1 prepares anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO22.8~
In 4.5V voltage ranges, with 0.5C rate charge-discharges, cycle performance curve graph.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail with attached drawing.
Embodiment 1
When the excessive amount of lithium and doped yttrium amount are respectively 10%, 0.02 (i.e. x=0.02), by weighing 1.1656g LiOH
H2O is dissolved in 10ml deionized waters, and 0.0565g Y are added2O3, grinding is uniform, adds 2.2852g presomas and anhydrous
Ethyl alcohol, grinding is until obtain the mixed slurry of rheology state, then continue to be ground under infrared lamp and go completely into mixed-powder；It puts again
Fine powder is dried and be ground into baking oven, and fine powder is finally put into tube furnace under oxygen atmosphere (oxygen gas flow rate 400ml/
Min 470 DEG C of pre-burning 6h) are warming up to the speed of 3 DEG C/min, then 780 DEG C of roasting 15h are warming up to the speed of 2 DEG C/min, then
450~500 DEG C are cooled to 2 DEG C/min programs, is finally cooled to the furnace product is levigate to get to Li after room temperature
(Ni0.8Co0.1Mn0.1)0.98Y0.02O2。
To the anode material for lithium-ion batteries Li (Ni of preparation0.8Co0.1Mn0.1)0.98Y0.02O2Carry out constant current charge-discharge survey
Examination, test result is as shown in Figure 2 to 7, from test result it can be seen that the positive electrode have high specific discharge capacity and
Very excellent stable circulation performance；Under room temperature environment, when voltage range is in 2.8~4.3V, constant current charge-discharge multiplying power is
When 0.5C, the first discharge specific capacity of the anode material for lithium-ion batteries can reach 180.4mAh g-1, after recycling 100 times still
It can reach 183.9mAh g-1, capacity retention ratio is up to 101.9%；When voltage range is in 2.8~4.5V, constant current charge-discharge times
When rate is 0.5C, the initial discharge specific capacity of the anode material for lithium-ion batteries can reach 192.0mAh g-1, cycle 100 times with
It still may be up to 189.4mAh g afterwards-1, capacity retention ratio 98.6%.
By respectively to the Li (Ni before doping0.8Co0.1Mn0.1)O2With the Li (Ni after doping0.8Co0.1Mn0.1)0.98Y0.02O2Material carries out surface residual alkali test, and LiOH contents are 0.27% before adulterating, and pH value 13.35, LiOH contains after doping
Amount is only 0.13%, pH value 12.53.
Embodiment 2
When the excessive amount of lithium and doped yttrium amount are respectively 5%, 0.02 (i.e. x=0.02), by weighing 1.1126g LiOH
H2O is dissolved in 10ml deionized waters, and 0.0565g Y are added2O3, grinding is uniform, adds 2.2852g presomas and anhydrous
Ethyl alcohol, grinding is until obtain the mixed slurry of rheology state, then continue to be ground under infrared lamp and go completely into mixed-powder；It puts again
The drying and levigate in baking oven, finally put it into tube furnace under oxygen atmosphere (oxygen gas flow rate 400ml/min) with 3 DEG C/
The speed of min is warming up to 470 DEG C of pre-burning 6h, then is warming up to 780 DEG C of roasting 15h with the speed of 2 DEG C/min, then with 2 DEG C/min journeys
Sequence is cooled to 450~500 DEG C, finally cools to the furnace product is levigate to get to Li (Ni after room temperature0.8Co0.1Mn0.1)0.98Y0.02O2。
To the anode material for lithium-ion batteries Li (Ni of preparation0.8Co0.1Mn0.1)0.98Y0.02O2Carry out constant current charge-discharge survey
Examination, from test result it can be seen that the positive electrode still has high specific discharge capacity and very excellent stable circulation performance；
Under room temperature environment, when voltage range is in 2.8~4.3V, when constant current charge-discharge multiplying power is 0.5C, the lithium ion cell positive
The first discharge specific capacity of material can reach 181.8mAh g-1, still can reach 183.4mAh g after recycling 100 times-1, capacity
Conservation rate is up to 100.9%；When voltage range is in 2.8~4.5V, when constant current charge-discharge multiplying power is 0.5C, the lithium ion battery
The initial discharge specific capacity of positive electrode can reach 192.5mAh g-1, 189.9mAh g are still may be up to after recycling 100 times-1,
Capacity retention ratio is 98.6%.
By respectively to the Li (Ni before doping0.8Co0.1Mn0.1)O2With the Li (Ni after doping0.8Co0.1Mn0.1)0.98Y0.02O2Material carries out surface residual alkali test, and LiOH contents are 0.16% before adulterating, and pH value 13.08, LiOH contains after doping
Amount is only 0.06%, pH value 11.73.
Embodiment 3
When the excessive amount of lithium and doped yttrium amount are respectively 10%, 0.01 (i.e. x=0.01), by weighing 1.1656g LiOH
H2O is dissolved in 10ml deionized waters, and 0.0283g Y are added2O3, grinding is uniform, adds 2.2509g presomas and anhydrous
Ethyl alcohol, grinding is until obtain the mixed slurry of rheology state, then continue to be ground under infrared lamp and go completely into mixed-powder；It puts again
The drying and levigate in baking oven, finally put it into tube furnace under oxygen atmosphere (oxygen gas flow rate 400ml/min) with 3 DEG C/
The speed of min is warming up to 470 DEG C of pre-burning 6h, then is warming up to 780 DEG C of roasting 15h with the speed of 2 DEG C/min, then with 2 DEG C/min journeys
Sequence is cooled to 450~500 DEG C, finally cools to the furnace product is levigate to get to Li (Ni after room temperature0.8Co0.1Mn0.1)0.99Y0.01O2。
To the anode material for lithium-ion batteries Li (Ni of preparation0.8Co0.1Mn0.1)0.99Y0.01O2Carry out constant current charge-discharge survey
Examination, from test result it can be seen that the positive electrode still has high specific discharge capacity and very excellent stable circulation performance；
Under room temperature environment, when voltage range is in 2.8~4.3V, when constant current charge-discharge multiplying power is 0.5C, the lithium ion cell positive
The first discharge specific capacity of material can reach 184.5mAh g-1, still can reach 184.9mAh g after recycling 100 times-1, capacity
Conservation rate is up to 100.2%；When voltage range is in 2.8~4.5V, when constant current charge-discharge multiplying power is 0.5C, the lithium ion battery
The initial discharge specific capacity of positive electrode can reach 195.6mAh g-1, 195.4mAh g are still may be up to after recycling 100 times-1,
Capacity retention ratio is 99.9%.
By respectively to the Li (Ni before doping0.8Co0.1Mn0.1)O2With the Li (Ni after doping0.8Co0.1Mn0.1)0.99Y0.01O2Material carries out surface residual alkali test, and LiOH contents are 0.27% before adulterating, and pH value 13.35, LiOH contains after doping
Amount is only 0.15%, pH value 12.62.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically
Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides
Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.
Claims (5)
1. anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2, which is characterized in that the lithium ion cell positive material
The biomolecule expressions of material are：Li(Ni0.8Co0.1Mn0.1)1-xYxO2, wherein 0<x≤0.05.
2. anode material for lithium-ion batteries Li (Ni0.8Co0.1Mn0.1)1-xYxO2Preparation method, which is characterized in that including following step
Suddenly：
Lithium source dissolution of raw material in deionized water, is added yttrium and expects to be uniformly mixed in a steady stream, grinding obtains mixed slurry by step 1.；
Ni is added in gained mixed slurry in step 1 by step 2. wherein0.8Co0.1Mn0.1(OH)2Presoma and absolute ethyl alcohol, after
Continuous grinding, until mixed slurry is abnormal in uniform flow, then continues to be ground to and goes completely into mixed-powder under infrared lamp；
Mixed-powder after grinding uniformly obtained by step 2 is placed in tube furnace under oxygen atmosphere first with 2~5 by step 3.
DEG C/min is warming up to 470~550 DEG C of 6~10h of pre-burning, then is warming up to 750~850 DEG C of 15~20h of roasting with 2~3 DEG C/min, then
450~500 DEG C are cooled to 2 DEG C/min programs, room temperature is finally cooled to the furnace, obtains Li (Ni0.8Co0.1Mn0.1)1-xYxO2。
3. by preparation method described in claim 2, which is characterized in that in step 1 and step 2, the lithium source raw material, yttrium source
The molar ratio of raw material and presoma is (1.10~1.20):x:(1-x).
4. by preparation method described in claim 2, which is characterized in that in step 1, the lithium source raw material is lithium carbonate, nitric acid
At least one of lithium, lithium acetate, lithium chloride and lithium hydroxide.
5. by preparation method described in claim 2, which is characterized in that in step 1, yttrium source raw material is yttrium nitrate, hydrogen-oxygen
Change at least one of the oxide of yttrium, yttrium sulfate, yttrium chloride and yttrium.
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| CN112366296A (en) * | 2020-09-30 | 2021-02-12 | 华中科技大学 | High-voltage-resistant lithium ion battery cathode material with layered structure and synthesis method and application thereof |
| CN112421014A (en) * | 2020-11-30 | 2021-02-26 | 蜂巢能源科技有限公司 | High-nickel ternary cathode material, preparation method thereof and lithium ion battery |
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