CN109860592A - A kind of nickel-cobalt lithium manganate cathode material and preparation method thereof of boracic molecular modification - Google Patents
A kind of nickel-cobalt lithium manganate cathode material and preparation method thereof of boracic molecular modification Download PDFInfo
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- CN109860592A CN109860592A CN201811590817.3A CN201811590817A CN109860592A CN 109860592 A CN109860592 A CN 109860592A CN 201811590817 A CN201811590817 A CN 201811590817A CN 109860592 A CN109860592 A CN 109860592A
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Abstract
The invention discloses a kind of nickel-cobalt lithium manganate cathode materials and preparation method thereof of boracic molecular modification, 4- vinylphenylboronic acid layer is linked at nickel-cobalt lithium manganate cathode material surface by covalent, the boron-containing group molecular layer of monolayer is formd on nickle cobalt lithium manganate powder surface, on material partial size itself without influence, and preparation method of the invention is implemented convenient for operation, modification temperature needed for preparation process is lower, time-consuming small, is suitable for industrialized production；In addition, the lithium ion battery battery chemical cycle performance of nickel-cobalt lithium manganate cathode material application preparation prepared by the present invention is significantly improved, capacity retention ratio and high rate performance are obviously improved.
Description
Technical field
The present invention relates to field of lithium ion battery more particularly to a kind of nickel-cobalt lithium manganate cathode materials of boracic molecular modification
And preparation method thereof.
Background technique
Demand with people to the lithium ion battery of high capacity and high power density is increasing, in recent years height ratio capacity
Material cause the great interest of people, and receive more and more attention.Especially have at low cost, toxicity it is low and it is high can
The nickelic LiNi of inverse capacity1-x-yCoxMnyO2Positive electrode (abbreviation NCM), it is considered to be conventional lithium ion battery positive electrode cobalt
The optimum substituent of sour lithium.
Nickelic LiNi1-x-yCoxMnyO2Material originates from LiNiO2, in base structure 80% reversible deintercalation can be utilized
Lithium, capacity are up to 220mAhg-1, relative to possessing about 140mAhg-1LiCoO2, LiNi1-x-yCoxMnyO2Material
With better lithium utilization rate.Co and Mn substitutes LiNiO2Middle part Ni greatly enhances the electric conductivity and knot of material
Structure stability.Most one of attractive nickelic LiNi1-x-yCoxMnyO2Material is LiNi0.8Co0.1Mn0.1O2(NCM), exist
0.1C charging and discharging currents, 4.3V blanking voltage under its specific discharge capacity be up to 200mAhg-1。
But sharply, in storage and cyclic process resistance increases and these insufficient disadvantages of thermal stability capacity attenuation, sternly
The commercial applications of this material are hindered again, on the surface of the material with the Ni of high activity4+The decomposition that can accelerate electrolyte, causes
Electrolyte consumption and the solid electrolyte membrane (SEI film) for forming thickness.Hindering another stubborn problem of NCM practical application is:
NCM material is quite sensitive to moisture, and which results in LiOH, LiOH and the CO in environment are formed on material surface2It is further anti-
The LiCO of insulation should be generated3, insulating layer is generated on the surface of the material.Therefore, NCM surface chemistries confrontation lithium ion battery material
Performance has conclusive influence.
There are researchers to pass through technological innovation at present to overcome these critical issues, surface cladding be improve NCM performance and
The common method of stability.These substances of metal fluoride, metal phosphate and metal oxide have been used for NCM nano surface
Layer cladding research.It is well known that clad can inhibit bad secondary anti-between material and electrolyte as physical protection layer
It answers, the corrosion of the HF in electrolyte can be slowed down.However accurately the thickness of control clad and uniformity difficulty are bigger.Pass through
The clad handled at high temperature after simply mixing with NCM presoma is usually non-uniform coarse cladding.In addition, Al2O3With
ZrO2These electrochemical properties and it is electroactive preferably, be often used as defence layer and carry out conventional cladding.Although concentration gradient material can
To solve this problem, but sacrifices part specific capacity and be inevitable.
Recent atomic layer deposition (ALD) technology is referred in the coating decoration of high-nickel material, is realized on positive electrode
Pin-free surface coating technology, the thickness of clad accurately control 0.1nm.However, expensive instrument and cumbersome operation
Process hinders answering on a large scale for this technology.
Therefore, well-designed and regulation is still needed in the surface coated controllable coating technology of high-nickel material.
Summary of the invention
Goal of the invention: in order to overcome defect existing in the prior art, the invention proposes a kind of boracic molecular modifications
Nickel-cobalt lithium manganate cathode material and preparation method thereof effectively improves the electricity of material by boracic molecular modification on positive electrode surface
Chemical property.
Technical solution: in order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows: a kind of boracic molecule is repaired
The nickel-cobalt lithium manganate cathode material of decorations, specially surface modification cladding chain are connected to the nickle cobalt lithium manganate anode of 4- vinylphenylboronic acid
Material.
Further, the surface modification cladding on-link mode (OLM) is the on-link mode (OLM) of covalent bond.
Further, the boracic molecule of the surface modification cladding is monolayer；Decorative layer is with a thickness of 1-5nm.
More preferably, the nickel-cobalt lithium manganate cathode material is nickle cobalt lithium manganate NCM811 material.
The invention also discloses the preparation method of the nickel-cobalt lithium manganate cathode material of above-mentioned boracic molecular modification, specific steps
Are as follows: nickel-cobalt lithium manganate cathode material and 4- vinylphenylboronic acid will be taken to be dissolved according to the ratio that mass ratio is 300:1-300:2
In acetone solvent, it is evenly stirred until dissolution completely, after reflux, filters out sediment and with oven drying after acetone washing 3 times, obtain
The LiNi modified to 4- vinylphenylboronic acid0.8Co0.1Mn0.1O2Powder can obtain the nickle cobalt lithium manganate anode of boracic molecular modification
Material.
More preferably, the whipping temp of the stirring is 55-65 DEG C.
More preferably, the return time is 10-13h.
More preferably, after the acetone washing, the drying temperature of oven drying is 75-85 DEG C；Drying time is 24-
26h。
The principle of the present invention is: 4- vinylphenylboronic acid layer is linked at nickel-cobalt lithium manganate cathode material by covalent
Surface, the boron atom in boryl anion receptor have high electrophilicity and electron deficient, and electron-withdrawing ability is strong, to change nickel
Cobalt manganic acid lithium Li Ni0.8Co0.1Mn0.1O2The surface nature of positive electrode；And then improve its chemical property.
The utility model has the advantages that nickel-cobalt lithium manganate cathode material and its preparation side of a kind of boracic molecular modification provided by the invention
4- vinylphenylboronic acid layer is linked at nickel-cobalt lithium manganate cathode material surface by covalent, in nickle cobalt lithium manganate by method
Powder surface forms the boron-containing group molecular layer of monolayer, on material partial size itself without influence, and preparation side of the invention
Method is implemented convenient for operation, and modification temperature needed for preparation process is lower, time-consuming small, is suitable for industrialized production；In addition, of the invention
The lithium ion battery battery chemical cycle performance of the nickel-cobalt lithium manganate cathode material application preparation of preparation is significantly improved, capacity
Conservation rate and high rate performance are obviously improved.
Detailed description of the invention:
Fig. 1 is the nickel-cobalt lithium manganate cathode material chemical structure signal of the boron molecular modification of 1-2 of embodiment of the present invention preparation
Figure；
Fig. 2 is that embodiment 1 and comparative example 1 are illustrated respectively as button cell electrochemistry cycle performance prepared by positive electrode
Figure；
Fig. 3 is that embodiment 2 and comparative example 1 are illustrated respectively as button cell electrochemistry cycle performance prepared by positive electrode
Figure.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail:
Embodiment 1:
A kind of preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification, the specific steps are as follows: by the nickel of 3g
The 4- vinylphenylboronic acid of cobalt manganic acid lithium NCM811 powder and 10mg are dissolved in acetone solvent, are evenly stirred until at 60 DEG C molten
Solution completely, flows back after 12h, filters out sediment and with acetone washing 3 times, then dries for 24 hours at 80 DEG C, obtains 4- vinyl
The modified LiNi0.8Co0.1Mn0.1O2 powder of phenyl boric acid, can obtain the nickel-cobalt lithium manganate cathode material of boracic molecular modification.
Embodiment 2:
A kind of preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification, the specific steps are as follows: by the nickel of 3g
The 4- vinylphenylboronic acid of cobalt manganic acid lithium NCM811 powder and 20mg are placed in acetone solvent to stir evenly at 65 DEG C, reflux
After 10h, sediment is filtered out and with acetone washing 3 times, then the dry 26h at 85 DEG C, it is modified to obtain 4- vinylphenylboronic acid
LiNi0.8Co0.1Mn0.1O2Powder can obtain the nickel-cobalt lithium manganate cathode material of boracic molecular modification.
Comparative example 1:
Not surface treated nickle cobalt lithium manganate NCM811 powder is as positive electrode.
Electrochemical property test test:
By the not surface treated nickle cobalt lithium manganate NCM811 powder of the embodiment 1-2 positive electrode prepared and comparative example 1
Button cell is prepared as follows into respectively as positive electrode in end:
The ratio that positive electrode, conductive agent, binder are 90:10:10 in mass ratio is sufficiently mixed, stirring is passed through
Uniform sizing material is made, is coated uniformly on aluminium foil, positive plate is cut into after dry and is dried in vacuo for 24 hours in 100 DEG C；With 1.0mol/L
LiPF6/ (EC+DMC+EMC) (EC, DMC, EMC volume ratio 1: 1: 1) is electrolyte, and lithium metal is to electrode, Cellgard-
2400 type polypropylene screens are diaphragm, are equipped to button cell in argon atmosphere glove box.
It is tested on LanHECT2001A type battery test system, charging/discharging voltage range is 2.8~4.3V
(vs.Li+/Li), as shown in Fig. 2-Fig. 3, Fig. 2 is the electrochemistry cyclicity of button cell prepared by embodiment 1 and comparative example 1
It can schematic diagram；Fig. 3 is the electrochemistry cycle performance schematic diagram of button cell prepared by embodiment 2 and comparative example 1；Other tests
The results are shown in Table 1:
Button cell performance test comparison prepared by 1 embodiment 1-2 of table and comparative example 1
| Test index | Embodiment 1 | Embodiment 2 | Comparative example 1 |
| The discharge capacity (mAh/g) of 0.1C | 200.2 | 200.5 | 199.8 |
| Discharge capacity (mAh/g) after 500C circulation | 169.3 | 171.9 | 150 |
| Capacity retention ratio | 84.5% | 85.7% | 75.1% |
As it can be seen from table 1 the button cell of the not surface treated nickle cobalt lithium manganate powder preparation of comparative example 1, passes through
After 500 circle circulations, discharge capacity 150mAh/g, capacity retention ratio 75.1%；And positive electrode prepared by the embodiment of the present invention 1
The button cell of preparation is after 500 circle circulations, discharge capacity 169.3mAh/g, capacity retention ratio 84.5%；Embodiment 2 is made
The button cell of standby positive electrode preparation is after 500 circle circulations, discharge capacity 171.9mAh/g, capacity retention ratio
85.7%.Compared to being greatly improved for comparative example 1.
A kind of nickel-cobalt lithium manganate cathode material and preparation method thereof of boracic molecular modification of the present invention, by 4- vinyl benzene boron
Acid layer is linked at nickel-cobalt lithium manganate cathode material surface by covalent, forms single point on nickle cobalt lithium manganate powder surface
The boron-containing group molecular layer of sublayer, lithium ion battery electrochemistry prepared by the nickel-cobalt lithium manganate cathode material application of preparation are followed
Ring performance is significantly improved, and capacity retention ratio and high rate performance are obviously improved.
Claims (8)
1. a kind of nickel-cobalt lithium manganate cathode material of boracic molecular modification, it is characterised in that coat chain for surface modification and be connected to 4- second
The nickel-cobalt lithium manganate cathode material of alkenyl phenyl boric acid.
2. the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 1, it is characterised in that the surface
Modification cladding on-link mode (OLM) is the on-link mode (OLM) of covalent bond.
3. the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 1, it is characterised in that: the surface
The boracic molecule of modification cladding is monolayer；Decorative layer is with a thickness of 1-5nm.
4. the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 1, it is characterised in that: the nickel cobalt
Manganate cathode material for lithium is nickle cobalt lithium manganate NCM811 material.
5. a kind of preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification described in claim 1, feature exist
In will according to mass ratio be 300:1-300:2 ratio take nickel-cobalt lithium manganate cathode material and 4- vinylphenylboronic acid to be dissolved in third
In ketone solvent, it is evenly stirred until dissolution completely, after reflux, filters out sediment and with oven drying after acetone washing 3 times, obtain
The modified LiNi of 4- vinylphenylboronic acid0.8Co0.1Mn0.1O2Powder can obtain the nickle cobalt lithium manganate anode material of boracic molecular modification
Material.
6. the preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 5, feature exist
In: the whipping temp of the stirring is 55-65 DEG C.
7. the preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 6, feature exist
In: the return time is 10-13h.
8. the preparation method of the nickel-cobalt lithium manganate cathode material of boracic molecular modification according to claim 7, feature exist
In: after the acetone washing, the drying temperature of oven drying is 75-85 DEG C；Drying time is 24-26h.
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| WO2021012708A1 (en) * | 2019-07-25 | 2021-01-28 | 苏州大学 | Siloxane modified high nickel metal oxide material and preparation method therefor |
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