CN101847722A - High-performance lithium ion battery cathode material and preparation method thereof - Google Patents
High-performance lithium ion battery cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lithium ion battery cathode material LiNixCoyM1-x-yO2 prepared from micron-sized single crystal particles and a preparation method thereof, wherein x is greater than 0 and is not more than 0.8, y is greater than 0 and is not more than 0.5, and M is one or two of Li, Mn, Al and Mg. The invention is characterized in that (1) composite oxide or hydroxide of transition metal nickel, transition metal cobalt and modified metal M is used as a raw material, the composite oxide or hydroxide is porous aggregate comprising nanocrystals, the average size of the aggregate is 2-50 micrometers, and the specific surface area of the aggregate is greater than 15m<2>/g (measured by BET method); (2) the composite metal oxide or hydroxide and lithium salts are milled in a ball mill, the micron-sized composite metal oxide or hydroxide is converted into nanocrystal particles to obtain a nano-sized mixed precursor of the composite metal oxide or hydroxide and the lithium salts, and the mixed precursor is sintered at uniform temperature to obtain the required lithium ion battery cathode material; and (3) the prepared lithium ion battery cathode material LiNixCoyM1-x-yO2 is basically prepared from micron-sized single crystal particles, and the average size of the single crystal particles is 2-20 micrometers. In addition, the product has excellent physical and electrochemical properties, such as ultra-low specific surface area, reasonable particle size distribution, good electrode processing properties, ultra-long cycle life, excellent rate capability, obvious high and low temperature cycling and storing properties and excellent safety; and the product can be widely used as a high-performance lithium ion battery cathode material. The invention provides the high-performance lithium ion battery cathode material and the preparation method thereof.
Description
Technical field
The present invention relates to a kind of secondary battery positive electrode material, particularly relate to a kind of lithium ion battery nickel and cobalt containing system layered cathode material.
Technical background
Phase early 1980s, people such as American scholar J.B.Goodenough have found cobalt acid lithium (LiCoO first
2), lithium nickelate (LiNiO
2) and LiMn2O4 (LiMn
2O
4) can be used as the material of removal lithium embedded ion, and applied for relevant patent.Wherein cobalt acid lithium is used in the lithium ion battery as positive electrode by the business-like first small-sized electronic product that is applied to of Sony corporation of Japan success in early 1990s with the chemical property of excellence and good electrode processing characteristics.Although lithium nickelate has very high reversible specific capacity (210mAh/g), structural stability that it is relatively poor and reasons such as thermal stability and synthetic difficulty can't be applied in practical lithium-ion.And the development of use for electronic products high-capacity lithium ion cell and power-type lithium ion battery is had higher requirement to positive electrode, as high reversible specific capacity, low cost and long circulation life and safe and reliable etc.Cobalt acid lithium is because shortcomings such as its limited reversible specific capacity, high cost and poor heat stability are not suitable as high performance lithium ion battery anode material of new generation.
The mid-90 in 20th century, people sight focused on have higher reversible specific capacity (＞180mAh/g) with the LiNi of lower price
0.8Co
0.2O
2In the research of positive electrode, and this material has also been obtained certain application in polymer Li-ion battery.But because positive electrode LiNi
0.8Co
0.2O
2There are shortcomings such as synthetic difficulty, thermal stability and structural stability difference, even the limited application in polymer Li-ion battery also needs and LiCoO
2Wait other positive electrode to mix and use, otherwise security performance can not get guaranteeing.Therefore, compound L iNi
0.8Co
0.2O
2Can not replace LiCoO
2And be widely used in anode material for lithium-ion batteries.
The positive electrode that at present is hopeful most to use in high performance lithium ion battery of new generation mainly contains modified spinelle manganic acid lithium (LiMn
2O
4), LiFePO 4 (LiFePO
4) and nickel-cobalt-manganese ternary system (Li (Ni, Co, Mn) O
2) material.LiFePO 4 (LiFePO
4) to have raw material sources abundant, cost is low, has extended cycle life, and structural stability and thermal stability advantages of higher, but its electronics and ionic conductivity are very low, make that this material high-rate charge-discharge capability and cryogenic property are relatively poor.In addition, also there is product stability in this material and shortcomings such as consistency is bad and tap density is low, electrode poor processability.
Mn is at the occurring in nature aboundresources, and positive spinel LiMn
2O
4The relative LiNiO of synthesis technique
2Also simple, thermal stability and overcharging resisting performance are better.Therefore, positive spinel LiMn
2O
4Be to be hopeful one of positive electrode that is applied to lithium ion battery of new generation most, the particularly application in high capacity lithium ion battery.But circulation and the shelf characteric of this material under high temperature (more than 55 ℃) is relatively poor, therefore, and with LiMn
2O
4For there are shortcomings such as serious self-discharge phenomenon and reversible capacity decay be too fast in the lithium ion battery of positive electrode active materials.
By at lithium nickel cobalt dioxide LiNi
xCo
1-xO
2In add other metallic element, can improve Stability Analysis of Structures, thermal stability and the cycle performance of this material.Prepare power-type lithium ion battery positive electrode LiNi as French Saft company by adding Al and Mg
0.8Co
0.15Al
0.05O
2And LiNi
0.8Co
0.15Mg
0.05O
2And, prepare nickel-cobalt-manganese ternary material (Li (Ni, Co, Mn) O by adding manganese
2).This ternary system positive electrode has higher specific capacity and structural stability and thermal stability preferably, but also has shortcoming such as the low and electrode poor processability of tap density.The nickle cobalt lithium manganate ternary material of preparation all is sphere or the spherical second particle of class that is gathered into by once little crystal grain both at home and abroad at present, and the tap density of material is lower, generally is lower than 2.4g/cm
3, the electrode filling capacity is bad, and when the electrode slice roll-in, second particle can break, and causes the contact between material and binding agent and the conductive agent bad, has influence on the compacted density of electrode and the chemical property of battery.
Obviously, existing positive electrode can not satisfy the instructions for use of use for electronic products high performance mini lithium ion battery and large capacity electric vehicle usefulness power-type lithium ion battery.Improve the actual specific capacity of positive electrode and improve cyclicity, must develop new positive electrode or existing material is carried out modification, to improve the chemical property of material.
Summary of the invention
The objective of the invention is to improve LiNi
xCo
yM
1-x-yO
2(0＜x≤0.8,0＜y≤0.5, M is Li, Mn, Al, the combination of a kind of among the Mg or two kinds) tap density, electrode processing characteristics, volume energy density, thus a kind of have high-energy-density and excellent cycle performance and safe and reliable micron single crystal granular anode material for lithium-ion batteries are provided.
Another object of the present invention is to provide the preparation method of this micron single crystal granular nickel and cobalt containing positive electrode.
The objective of the invention is to realize by the following technical solutions:
The invention provides a kind of nickel and cobalt containing positive electrode, can with electrolyte solution or solid electrolyte, and negative active core-shell material forms lithium ion battery together, it is characterized in that this nickel and cobalt containing positive electrode is the LiNi with layer structure structure
xCo
yM
1-x-yO
2(0＜x≤0.8,0＜y≤0.5, M is Li, Mn, Al, the combination of a kind of among the Mg or two kinds).
The invention provides a kind of preparation method of described nickel and cobalt containing positive electrode, comprise the steps:
1) with the composite oxides of nickel cobalt and modified metal M and lithium salts by Li/ (Mn+M)=1.0～1.1: 1 mol ratio ball milling mixes;
2) pressed powder that step 1) is made was heat-treated 1～48 hour under 400～1200 ℃, and sintering makes lithium ion battery nickel and cobalt containing positive electrode.
Modified metal M in the described step 1) is Li, Mn, Al, the combination of a kind of among the Mg or two kinds.
The porous micron order aggregate that the nickel cobalt in the described step 1) and the composite oxides of modified metal M or hydroxide are made up of nano microcrystalline, this aggregate average-size is between the 1-20 micron, and the composite oxide power specific area is greater than 15m
2/ g.
Lithium salts in the described step 1) comprises Li
2CO
3, LiOHH
2O, LiNO
3, CH
3COOLi.
The composite oxides of the nickel in the described step 1), cobalt and modified metal M or hydroxide micron order aggregate change the nano microcrystalline particle into after grinding, become the mixing presoma with nano-scale behind the lithium salts ball milling.
Described step 2) optimal sintering temperature in is 850-1150 ℃, and best sintering time is 10-24 hour.
The preparation method of nickel and cobalt containing positive electrode provided by the invention, mainly be by selecting for use nickel cobalt and modified metal M to have porous composite oxide that nano microcrystalline forms or hydroxide as raw material, prepare presoma through behind the abundant ball milling with nano-scale, high temperature sintering is prepared the modification nickel and cobalt containing positive electrode with micron single crystal granular then, improved the tap density of material, electrode processing characteristics and high-rate charge-discharge capability, thereby the energy density and the high power output performance of raising battery.
The invention provides the nickel and cobalt containing positive electrode active materials as lithium ion battery, have the tap density height, the electrode good processability has extended cycle life, remarkable advantages such as security performance excellence.In addition, the complete and ganoid micron single crystal granular that product has can improve the electrode processing characteristics of material, has improved the compacted density of electrode.Complete and the orderly mono-crystalline structures of growing has regular and three-dimensional channel lithium ion motion smoothly, reduced the obstruction of in the charge and discharge process lithium ion being moved, thereby make this material have the ultra-high magnifications charge-discharge performance, be more suitable in high power type lithium ion batteries such as electric tool and hybrid electric vehicle, using.
Description of drawings
Fig. 1 is the LiNi in the embodiment of the invention 1
0.35Co
0.3Mn
0.35O
2Sweep and do electron micrograph (SEM);
Fig. 2 is the LiNi in the embodiment of the invention 1
0.35Co
0.3Mn
0.35O
2X-ray diffractogram (XRD);
Fig. 3 is LiNi in the embodiment of the invention 1
0.35Co
0.3Mn
0.35O
2Preceding 100 all charging and discharging curves;
Fig. 4 is the laser particle size distribution curve of preparation powder body material in the embodiment of the invention 1;
Embodiment
Below in conjunction with the drawings and Examples card the present invention is further illustrated.
Composite oxides presoma (Ni: Co: Mn=0.35: 0.3: 0.35) and 26 kilograms of Li with 50 kilograms of nickel cobalts and manganese
2CO
3Abundant ground and mixed, presintering 5 hours under 450 degree then is warmed up to 950 degree high temperature sintering 24 hours down, last cool to room temperature then.
The granular size of material and morphology observation are carried out on Hitachi S-4000 electronic scanner microscope.We can find from Fig. 1, the novel LiNi of our preparation
0.35Co
0.3Mn
0.35O
2Be single crystal grain, average grain size about the 5-10 micron, even particle size, smooth surface.
The crystal structure of material adopts Rigaku B/Max-2400X x ray diffractometer x (Rigaku Ltd.) to analyze, and Cu K α line is a light source, and the angle of diffraction 2 θ are from 10 ° to 90 °.We can find from Fig. 2, and synthetic material has the layer structure of standard, and free from admixture exists mutually.
The specific area of the synthetic material that the Flow Sorb III that utilizes BET method mensuration to use U.S. Merck ﹠ Co., Inc to produce measures is 0.4m
2/ g.
In order to measure the chemical property of this material, above-mentioned synthetic electroactive substance, acetylene black and PVDF (Kynoar) are mixed the formation slurry at normal temperatures and pressures according to 85: 10: 5 ratio, evenly be coated on the aluminum substrates. with the electrode slice that obtains at 140 ℃ down after the oven dry, under certain pressure, compress, continuation was dried 12 hours down at 140 ℃, and then film being cut into area is 1cm
2Thin rounded flakes as positive pole.With the pour lithium slice is negative pole, thinks 1mol/l LiPF
6EC+DMC (volume ratio 1: 1) electrolyte is assembled into Experimental cell in being full of the glove box of argon gas.
Experimental cell is tested by being subjected to computer-controlled auto charge and discharge instrument to carry out charge and discharge cycles.Charging and discharging currents is 20mA/g, and the charging cut-ff voltage is 4.3V, and discharge cut-off voltage is 2.5V, and 2～5 charging and discharging curves as shown in Figure 3.
Fig. 4 is the laser particle size distribution curve of the preparation powder body material of mensuration, and as can be seen from the figure, the material granule of preparation presents normal distribution.
By preparation method of the present invention synthetic a series of stratiform structure LiNi under different condition
xCo
yM
1-x-yO
2Positive electrode active materials
According to preparation method provided by the invention, under the listed different condition of table 1, synthetic a series of stratiform structure LiNi
xCo
yM
1-x-yO
2Positive electrode active materials.
Table 1
| Embodiment | Chemical composition | Composite oxides or hydroxide | Lithium salts | Reversible specific capacity (mAh/g) |
| ??2 | ??LiNi 0.5Co 0.2Mn 0.3O 2 | ??NiO-Mn 3O 4-Co 3O 4 | Lithium carbonate | ?165 |
| ??3 | ??LiNi 0.7Co 0.2Al 0.1O 2 | ??Mn 3O 4-CoO-Al 2O 3 | Lithium nitrate | ?168 |
| ???4 | ??LiNi 0.5Co 0.15Mg 0.05O 2 | ??Co(OH) 2-Ni(OH) 2-Mg(OH) 2 | Lithium hydroxide | ?162 |
| ??5 | ??LiNi 0.4Co 0.2Mn 0.3Al 0.1O 2 | ??MnO 2-Co 3O 4-NiO-Al 2O 3 | Lithium carbonate | ?150 |
| ??6 | ??LiNi 0.5Co 0.2Mn 0.25Mg 0.05O 2 | ??MnO 2-Co 3O 4-NiO-Al 2O 3 | Lithium carbonate | ?145 |
| ??7 | ??LiNi 0.4Co 0.2Mn 0.4O 2 | ??Co(OH) 2-Ni(OH) 2-Mn(OH) 2 | Lithium hydroxide | ?156 |
| ??8 | ??LiNi 0.4Co 0.15Mn 0.4Li 0.05O 2 | ??Mn 3O 4-MgO-NiO | Lithium carbonate | ?154 |
| ??9 | ??LiNi 0.7Co 0.2Al 0.06Li 0.04O 2 | ??Mn 3O 4-CoO-Al 2O 3 | Lithium hydroxide | ?178 |
Embodiment 11,
Complex hydroxide presoma and 27.4 kilograms of lithium hydroxides of 50 kilograms of nickel cobalt manganese and aluminium are mixed, abundant then ball milling, presintering 8 hours under 400 degree then, be warmed up to the following high temperature sintering of 850 degree 24 hours then, last cool to room temperature synthesizes needed lithium ion battery nickel and cobalt containing layer structure positive electrode active materials.
Claims (5)
1. the positive electrode of a nickeliferous and cobalt, can with electrolyte solution or solid electrolyte, and negative active core-shell material forms lithium ion battery together, it is characterized in that this positive electrode is that chemical formula can be expressed as LiNi
xCo
yM
1-x-yO
2(0＜x≤0.8,0＜y≤0.5, M is Li, Mn, Al, the combination of a kind of among the Mg or two kinds).
2. the preparation method of a nickeliferous according to claim 1 and cobalt positive electrode comprises the steps:
1) with the composite oxides of nickel, cobalt and modified metal M or hydroxide and lithium salts by Li/ (Co+Ni+M)=1.0～1.2: 1 mol ratio ball milling mixed 1～10 hour;
2) the mixing presoma that step 1) is made was heat-treated 1～48 hour under 400～1200 ℃, and sintering makes the manganese anode material that contains that lithium ion battery uses.
3. the preparation method of positive electrode as claimed in claim 2, it is characterized in that, the porous aggregate that the composite oxides of the nickel in the described step 1), cobalt and modified metal M or hydroxide are made up of nano microcrystalline, this aggregate average-size is between the 2-50 micron, and composite oxides or hydroxide powder specific area are greater than 15m
2/ g (BET method mensuration).
4. the preparation method of positive electrode as claimed in claim 2, it is characterized in that, the composite oxides of the nickel in the described step 1), cobalt and modified metal M or hydroxide micron order aggregate change the nano microcrystalline particle into after grinding, become the mixing presoma with nano-scale behind the lithium salts ball milling.
5. nickeliferous, cobalt positive electrode as claimed in claim 1 is characterized in that this material is made up of micron single crystal granular basically, and the single crystal grain average-size is between the 2-20 micron.
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| CN102054976A (en) * | 2010-12-10 | 2011-05-11 | 王志勇 | Preparation method of lithium ion battery cathode material |
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| CN104241640A (en) * | 2014-10-10 | 2014-12-24 | 国家电网公司 | Lithium nickel-cobalt-aluminum positive electrode material, preparation method thereof and lithium ion battery |
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