CN110492067A - A kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material - Google Patents
A kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material Download PDFInfo
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- CN110492067A CN110492067A CN201910708118.2A CN201910708118A CN110492067A CN 110492067 A CN110492067 A CN 110492067A CN 201910708118 A CN201910708118 A CN 201910708118A CN 110492067 A CN110492067 A CN 110492067A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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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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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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 preparation method that the present invention provides a kind of aluminium titanium compound coating nickel cobalt manganese anode material includes the following steps, the nickel cobalt manganese anode material that preparation is completed is placed in settling chamber, using Bubbling method by carrier gas by two evaporators aluminium secondary butylate and titanium tetraisopropylate bring the settling chamber into respectively, and carrier gas is passed through to settling chamber, after reacting a period of time at 250 ~ 350 DEG C of deposition chamber temperatures, close carrier gas, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, and aluminium titanium compound coating nickel cobalt manganese anode material can be obtained.The present invention can directly prepare aluminium titanium compound coating nickel cobalt manganese anode material under the conditions of relatively low temperature, covered effect uniformly, compositely proportional and film forming thickness it is easily-controllable, simple process.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of preparation of aluminium titanium compound coating nickel cobalt manganese anode material
Method.
Background technique
The scarcity of earth energy and people improve environmental protection consciousness, and new-energy automobile is widelyd popularize in recent years,
The lithium-ion-power cell used is also rapidly developed therewith.In new-energy automobile and the competition of conventional fuel oil automobile, battery energy
Metric density is to restrict its universal one of bottleneck.Positive electrode of the nickel cobalt manganese material as current highest energy density, market part
Volume speedup has reached highest, it has also become lithium-ion-power cell hot topic positive electrode.
Improve nickel cobalt manganese anode material cycle life, high rate performance and coulombic efficiency for the first time, coating modification scheme to improve
Obtain good improvement.Covering material is numerous, such as aluminium oxide, zirconium oxide, titanium oxide, magnesia, these materials by
Prove that there is the characteristic for improving positive electrode cycle performance.It is believed that these metal oxides in charge and discharge process, obstruct
Positive active material is directly contacted with electrolyte, avoids active material by electrolytic corrosion；To improve positive electrode
Stability, realize the promotion of cycle life.
Currently, most common method for coating is liquid phase coating method, the metal salt solution of blended anode material and preparation and
Corresponding deposition agent, then after being evaporated, be filtered, washed, being heat-treated, the positive electrode being covered to complete.Such methods are past
Toward complex steps, covered effect is not uniform enough the defects of, influence the promotion of positive electrode performance.
Summary of the invention
It is above-mentioned to overcome the object of the present invention is to provide a kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material
Technical problem.
Above-mentioned technical purpose of the invention technical scheme is that:
A kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material includes the following steps, the nickel cobalt that preparation is completed
Manganese anode material is placed in settling chamber, passes through carrier gas for the aluminium secondary butylate and titanium tetraisopropylate in two evaporators using Bubbling method
It brings the settling chamber into respectively, and is passed through carrier gas to settling chamber, a period of time is reacted at 250~350 DEG C of deposition chamber temperatures
Afterwards, carrier gas is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, aluminium titanium compound coating nickel cobalt can be obtained
Manganese anode material.
The further technical solution of the present invention is, by the carrier gas flux A that aluminium secondary butylate brings settling chamber into be 0.4~
The carrier gas flux B that the titanium tetraisopropylate brings settling chamber into is 0.1~0.3slm by 0.6slm, and the flow of the carrier gas is
1.5~2.5slm.
The further technical solution of the present invention is that the carrier gas and carrier gas are one of inert gas.
The further technical solution of the present invention is that the carrier gas and carrier gas are high pure nitrogen.
The further technical solution of the present invention is, the carrier gas flux A, carrier gas flux B and dilution air flow measurer have with
Lower relationship: 1:0.2~0.4:3~6.
The further technical solution of the present invention is that the aluminium secondary butylate, titanium tetraisopropylate and nickel cobalt manganese anode material exist
Depositing the indoor reaction time is 5~15min.
The further technical solution of the present invention is that the temperature of the evaporator is controlled at 120~130 DEG C, by the Zhong Ding
The carrier gas passage temperature that aluminium alcoholates and titanium tetraisopropylate bring the settling chamber into respectively is controlled at 90~110 DEG C.
The utility model has the advantages that the present invention can directly prepare aluminium titanium compound coating nickel cobalt manganese anode material under the conditions of relatively low temperature
Material, covered effect uniformly, compositely proportional and film forming thickness it is easily-controllable, simple process.
Detailed description of the invention
Fig. 1 is aluminium titanium compound coating nickel cobalt manganese anode material obtained by embodiment 1-4 in 2.8-4.2V voltage range, 1C multiplying power
Under cycle performance curve.
Specific embodiment
In the description of the present invention, unless otherwise indicated, the side of the instructions such as term " on " "lower" " left side " " right side " " preceding " " rear "
Position or positional relationship are merely to describing the present invention and simplifying description, rather than the device of indication or suggestion meaning or structure are necessary
With specific orientation, therefore it is not considered as limiting the invention.In addition, term " first " " second " etc. is only used for describing
Purpose is not understood to indicate or imply relative importance.
As shown in Figure 1, a kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material of the present invention include with
The nickel cobalt manganese anode material that preparation is completed is placed in settling chamber by lower step, using high pure nitrogen as carrier gas, using Bubbling method by two
Aluminium secondary butylate and titanium tetraisopropylate in a evaporator bring the settling chamber into respectively, wherein the temperature control of the evaporator exists
120~130 DEG C, the carrier gas passage temperature that the aluminium secondary butylate and titanium tetraisopropylate bring the settling chamber into respectively is controlled 90
~110 DEG C, it is 0.4~0.6slm by the carrier gas flux A that aluminium secondary butylate brings settling chamber into, brings the titanium tetraisopropylate into deposition
The carrier gas flux B of room is 0.1~0.3slm；It is passed through carrier gas to settling chamber simultaneously, the carrier gas uses high pure nitrogen or height
Pure argon, flow are 1.5~2.5slm, and further, the carrier gas flux A, carrier gas flux B and dilution air flow measurer have
Following relationship: 1:0.2~0.4:2.5~5；Deposition chamber temperatures are adjusted to 250~350 DEG C, make aluminium secondary butylate and with four isopropyls
Alcohol titanium thermally decomposes to generate aluminium oxide and titanium oxide in settling chamber and compound coating is at nickel cobalt manganese anode material surface, reaction
Between be 5~15min；After reaction, carrier gas is closed, keeps carrier gas flow until deposition chamber temperatures drop to 100 DEG C or 100
DEG C hereinafter, aluminium titanium compound coating nickel cobalt manganese anode material can be obtained.
Embodiment 1
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.6slm and 0.2slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 2slm；(2) be pre-placed in settling chamber to
The nickel cobalt manganese anode material of coating, and carry out vacuumize process, at 300 DEG C of depositing temperature, aluminium secondary butylate and with four isopropanols
Titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 6min；(3) anti-
At the end of answering, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, obtains the compound packet of aluminium titanium
Cover nickel cobalt manganese anode material.
Embodiment 2
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.6slm and 0.2slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 2slm；(2) be pre-placed in settling chamber to
The nickel cobalt manganese anode material of coating, and carry out vacuumize process, at 300 DEG C of depositing temperature, aluminium secondary butylate and with four isopropanols
Titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 10min；(3) anti-
At the end of answering, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, obtains the compound packet of aluminium titanium
Cover nickel cobalt manganese anode material.
Embodiment 3
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.6slm and 0.2slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 2slm；(2) be pre-placed in settling chamber to
The nickel cobalt manganese anode material of coating, and carry out vacuumize process, at 300 DEG C of depositing temperature, aluminium secondary butylate and with four isopropanols
Titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 20min；(3) anti-
At the end of answering, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, obtains the compound packet of aluminium titanium
Cover nickel cobalt manganese anode material.
Embodiment 4
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.6slm and 0.2slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 2slm；(2) be pre-placed in settling chamber to
The nickel cobalt manganese anode material of coating, and carry out vacuumize process, at 300 DEG C of depositing temperature, aluminium secondary butylate and with four isopropanols
Titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 15min；(3) anti-
At the end of answering, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, obtains the compound packet of aluminium titanium
Cover nickel cobalt manganese anode material.
Embodiment 5
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.4slm and 0.3slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 1.5slm；(2) it is pre-placed in settling chamber
Nickel cobalt manganese anode material to be coated, and carry out vacuumize process, at 350 DEG C of depositing temperature, aluminium secondary butylate and with four isopropyls
Alcohol titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 15min；(3)
At the end of reaction, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, it is compound to obtain aluminium titanium
Coat nickel cobalt manganese anode material.
Embodiment 6
(1) using high pure nitrogen as carrier gas, by Bubbling method respectively by two evaporators aluminium secondary butylate and with four isopropyls
Alcohol titanium brings settling chamber into, and carrier gas flux corresponds to 0.6slm and 0.3slm, and evaporator temperature is controlled at 125 DEG C, carrier gas passage
Temperature is maintained at 100 DEG C, while being passed through carrier gas to settling chamber, and carrier gas flow is 2.5slm；(2) it is pre-placed in settling chamber
Nickel cobalt manganese anode material to be coated, and carry out vacuumize process, at 250 DEG C of depositing temperature, aluminium secondary butylate and with four isopropyls
Alcohol titanium thermally decomposes to generate aluminium oxide and titanium oxide, and compound coating is in nickel cobalt manganese anode material surface, reaction time 5min；(3)
At the end of reaction, carrier gas flux is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, it is compound to obtain aluminium titanium
Coat nickel cobalt manganese anode material.
Comparative example 1
Uncoated nickel cobalt manganese anode material.
By X-ray fluorescence spectra analysis to the aluminium titanium compound coating nickel cobalt manganese anode material of embodiment 1-6 and comparative example 1
Covering amount detected, testing result such as following table.
From in upper table it is found that temperature be 250~350 DEG C between when covering amount it is relatively stable, and when temperature is lower sink
Product interior is hardly reacted, and when temperature is higher, reaction is too fast, is had aluminium oxide and titanium oxide to generate in the gas phase of settling chamber and is fallen
Positive electrode surface is fallen on, cladding can not be played the role of；Simultaneously to 1 gained aluminium titanium compound coating of embodiment 1-3 and comparative example
Cycle performance of the nickel cobalt manganese anode material under the 1C multiplying power of 2.8-4.2V voltage range is detected, testing result such as Fig. 1 institute
Show, it can be seen that aluminium titanium compound coating made from this law is modified nickel cobalt manganese anode material, covers nickel cobalt manganese anode with uncoated
Material is compared, and the anode material discharging platform after cladding is more gentle, has more stable cycle performance, and from Fig. 1 and implementation
When the reaction time is in 5-15min, performance is better than comparative example 1 known in example 1-4, and obtained product when covering amount is 0.5%
Cycle performance is optimal.
In order to keep the objectives, technical solutions, and advantages of the present invention more concise, present invention embodiments above
It is illustrated, is used only to describe the present invention, should not be understood as limiting the scope of the present invention.It should be pointed out that it is all
Any modifications, equivalent replacements, and improvements etc. done within the spirit and principles in the present invention, should be included in protection of the invention
Within the scope of.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of preparation method of aluminium titanium compound coating nickel cobalt manganese anode material, which is characterized in that include the following steps, will prepare
The nickel cobalt manganese anode material of completion is placed in settling chamber, using Bubbling method by carrier gas by two evaporators aluminium secondary butylate and
Titanium tetraisopropylate brings the settling chamber into respectively, and is passed through carrier gas to settling chamber, reacts at 250 ~ 350 DEG C of deposition chamber temperatures
After a period of time, carrier gas is closed, holding carrier gas flow drops to 100 DEG C up to deposition chamber temperatures, it is compound that aluminium titanium can be obtained
Coat nickel cobalt manganese anode material.
2. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as described in claim 1, which is characterized in that by Zhong Ding
The carrier gas flux A that aluminium alcoholates brings settling chamber into is 0.4 ~ 0.6 slm, and the titanium tetraisopropylate is brought into the carrier gas flux B of settling chamber
For 0.1 ~ 0.3 slm, the flow of the carrier gas is 1.5 ~ 2.5 slm.
3. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as claimed in claim 1 or 2, which is characterized in that institute
It states carrier gas and carrier gas is one of inert gas.
4. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as claimed in claim 3, the carrier gas and carrier gas
It is high pure nitrogen or high-purity argon gas.
5. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as claimed in claim 2, which is characterized in that the load
Throughput A, carrier gas flux B and dilution air flow measurer have following relationship: 1:0.2 ~ 0.4:3 ~ 6.
6. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as described in claim 1, which is characterized in that described secondary
Aluminium butoxide, titanium tetraisopropylate and nickel cobalt manganese anode material are 5 ~ 15min depositing the indoor reaction time.
7. the preparation method of aluminium titanium compound coating nickel cobalt manganese anode material as described in claim 1, which is characterized in that the steaming
The temperature for sending out device is controlled at 120 ~ 130 DEG C, and the aluminium secondary butylate and titanium tetraisopropylate are brought into the carrier gas of the settling chamber respectively
Channel temperature is controlled at 90 ~ 110 DEG C.
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Cited By (3)
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| CN111525109A (en) * | 2020-04-26 | 2020-08-11 | 陕西红马科技有限公司 | Preparation method of layered nickel-manganese binary positive electrode material coated with titanium-cobalt coating |
| WO2021082314A1 (en) * | 2019-10-29 | 2021-05-06 | 蜂巢能源科技有限公司 | Lithium-ion battery positive electrode material and preparation method therefor |
| CN114759183A (en) * | 2022-05-30 | 2022-07-15 | 远景动力技术(江苏)有限公司 | Low-cobalt positive electrode active material, method for producing same, electrochemical device, and electronic device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021082314A1 (en) * | 2019-10-29 | 2021-05-06 | 蜂巢能源科技有限公司 | Lithium-ion battery positive electrode material and preparation method therefor |
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| CN114759183A (en) * | 2022-05-30 | 2022-07-15 | 远景动力技术(江苏)有限公司 | Low-cobalt positive electrode active material, method for producing same, electrochemical device, and electronic device |
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