CN107845807A - A kind of preparation method of Manganese Based Cathode Materials for Lithium Ion Batteries - Google Patents
A kind of preparation method of Manganese Based Cathode Materials for Lithium Ion Batteries Download PDFInfo
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- CN107845807A CN107845807A CN201711043756.4A CN201711043756A CN107845807A CN 107845807 A CN107845807 A CN 107845807A CN 201711043756 A CN201711043756 A CN 201711043756A CN 107845807 A CN107845807 A CN 107845807A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides the method that a kind of using plasma enhancing chemical vapor deposition (PECVD) technology prepares Manganese Based Cathode Materials for Lithium Ion Batteries.Its method is first to prepare the presoma containing manganese of doping vario-property, then by presoma and lithium salts ball milling mixing it is uniform after, it is placed in plasma enhancing rotary furnace, and it is continually fed into oxygen-containing gas, plasma discharge is produced the active oxygen ion moved freely by optimizing device parameter, synthesize manganese-based anode material.The manganese-based anode material prepared by this method has that synthesis temperature is low, generated time is short, material homogeneity is good, form is regular, granularity is small, it is easy to cladding and doping vario-property, specific discharge capacity and multiplying power stability significantly improve, suitable for lithium-ion-power cell application field.
Description
Technical field
The invention belongs to lithium-ion-power cell application field, more particularly to a kind of using plasma enhancing chemical gaseous phase
The method that deposition (PECVD) technology prepares Manganese Based Cathode Materials for Lithium Ion Batteries.
Background technology
Lithium ion battery has that operating voltage is high, have extended cycle life, specific energy density is big, the protrusion such as environmentally friendly is excellent
Point, the fields such as electric tool, medicine equipment and digital product have been widely applied to it.In recent years, going out with new energy policy
Platform and lithium ion battery key technology develop rapidly, and motive-power battery turns into one of most hotly competitive product of in the market.Manganese
Base anode material typically refers to LiMn2O4, nickel ion doped, lithium-rich manganese-based anode material, and because having, raw material sources are extensive, energy is close
Degree and power density height, good rate capability, cheap, easy the advantages that reclaiming, be environmentally friendly, it is considered to be most develop
One of lithium ion power battery cathode material of prospect.
The preparation method of manganese-based anode material is a lot, and solid phase method is the most commonly used method of current merchandized handling.But pass
The solid phase method of system can only realize the other mixing of molecular level by ball mill mixing, during roasting the granule size of material whard to control and point
Cloth, it is difficult to prepare be uniformly dispersed, the sample that uniformity is good.Therefore the preparation side that a kind of reaction temperature is low, speed is fast is sought
Method is most important.
Plasma is often known as the state of material the 4th in addition to gaseous state, liquid, solid-state, has some conventional senses
The advantageous property that can not be obtained, the intensive treatment of material surface performance is commonly used in, treatment temperature can be reduced, accelerate processing speed
Degree, improve processing quality, enhancing reinforcing effect, reduce processing cost, elongated component service life.
Rarely have document report using plasma enhancing chemical vapor deposition (PECVD) technology to prepare manganese-based anode material at present
Material, can efficiently solve Mn2+The cation mixing problem caused by oxidation is insufficient in roasting process.Chinese patent
CN104659355A discloses a kind of preparation method and applications of spinel lithium manganate, comprises the following steps：Weigh lithium source and
Manganese source, it is dissolved in easy volatile solvent, stirring ball-milling, dries, be put into plasma tubular type stove, lead to oxygen, then carries out taking out very
Sky, at the uniform velocity heat up, heat (500 DEG C), carry out corona treatment, be then at the uniform velocity cooled to room temperature, that is, obtain spinel manganese acid
Lithium.The patent uses Low Temperature Solid-Phase plasma-assisted process synthetic spinel LiMn2O4, overcomes the conjunction of traditional industry high temperature solid-state
Into in method, high energy consumption caused by high temperature, it is longer to high request and the generated time of equipment the shortcomings of, and the preparation method
Have the characteristics that manufacture method is simple and convenient to operate, cost is cheap, beneficial to industrialized production.But the spinel lithium manganate prepared
Specific capacity and cycle performance are still relatively low first, it is difficult to meet the requirement of high performance lithium ion battery.
Chinese patent CN106992296A disclose electromagnetic field containment of the nickelic positive electrode of a kind of lithium ion battery etc. from
Daughter oxidation method of roasting, it is uniformly to mix presoma and lithium source powder, is placed in calciner and is calcined (800
DEG C), oxygen-containing gas is continually fed into, the oxygen-containing gas is produced positively charged active oxygen by plasma discharge, passes through
Applying electromagnetic field in the calciner makes the motion of the active oxygen deflect, and constraint is enriched in presoma and lithium source powder
Near body, nickelic positive electrode is synthesized.The patent can be by the use of lithium carbonate as lithium source, and synthesis performance is excellent in air atmosphere
Nickelic positive electrode, significantly reduce material and prepare cost.But it needs deflection electromagnetic field to enter row constraint to active oxygen, and need to be to existing
There is equipment to be transformed, manufacturing process is complex.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of method for preparing Manganese Based Cathode Materials for Lithium Ion Batteries, first made
The presoma containing manganese of standby doping vario-property, reach manganese with adulterating the mixing of high volence metal ion on a molecular scale, and then synthesize knot
Brilliant degree is high, the Mn of particle fine uniformxMyOzPresoma, plasma treatment technique is recycled to prepare manganese-based anode material.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of using plasma enhancing chemical vapor deposition (PECVD) technology prepares Manganese Based Cathode Materials for Lithium Ion Batteries
Method, including：
The presoma containing manganese of doping vario-property is first prepared using co-electrodeposition method, is well mixed with lithium salts, in oxygen active particles
High-temperature process, cooling, produce manganese-based anode material under plasma existence condition.
Existing Low Temperature Solid-Phase plasma-assisted process synthetic spinel LiMn2O4 has the advantages of low energy consumption, efficiency high,
But its high rate performance and cycle performance are still relatively low, it is difficult to meet the requirement of high performance lithium ion battery.It is therefore, of the invention
Wish further to lift its capacity and cycle performance by the modification to manganese source.In research, the application has mainly attempted surface
Cladding and atom doped both direction.Wherein, found during carbon coating (sucrose is raw material) is carried out：Due to plasma
Enhancing rotary furnace contain substantial amounts of oxygen active particles (including：O+、O2 +、O3 +) plasma, sucrose is completely converted into CO2, nothing
Method realizes Surface coating.Therefore, the present invention transfers to mix by the way of atom doped, and to doped chemical and lithium source, manganese source
Conjunction mode, process conditions carry out system and grope and study, the results showed that：Compared with other doping methods, co-electrodeposition method doping
The manganese-based anode material that modified presoma containing manganese is prepared with lithium source in plasma rotary furnace, have higher forthright again
Energy, cycle performance and crystallinity.
Preferably, in the presoma containing manganese and lithium salts, Mn:The mol ratio of Li elements is 1：1.
It also found in the application research：Although plasma can reduce the temperature of solid phase method, with oxygen active particles
The increase of plasma content, the quantity of side reaction and accessory substance can be also increased slightly in reaction.Particularly, after doping vario-property
Manganese source, because the increase of element species, this phenomenon are even more serious.Therefore, the present invention is mixed manganese source using co-electrodeposition method
Miscellaneous modification, using this method product purity it is high the characteristics of, reduce side reaction in solidification process, and the production of metastable state non crystalline structure
Raw, obtained positive electrode has more accurately stoichiometric proportion, more high rate capability, cycle performance and crystallinity.
Therefore, the preparation method of the currently preferred presoma containing manganese is：Using manganese source, alkali lye and doped chemical as original
It is prepared by material, co-electrodeposition method.
It is furthermore preferred that the manganese source compound is MnCl2、MnO2、MnSO4、Mn(NO3)2、(CH3COO)2Mn and MnC2O4In
One or more；
It is furthermore preferred that described alkali lye is ammoniacal liquor, NaOH, KOH and Na2CO3In one or more；
It is furthermore preferred that the doped chemical is one kind or several in Al, Se, Mg, Zn, Co, Ti, Ni, Fe, V, Cr, S, P
Kind.
Preferably, the lithium salts is Li2CO3、LiOH、CH3COOLi and Li2C2O4In one or more.
Preferably, the pressure of the oxygen-containing gas is 50~100pa, 0.01~10L/min of feed rate.
Preferably, the oxygen-containing gas is the one or more in oxygen-enriched air, purity oxygen and air.
Preferably, the frequency of the plasma enhancing rotary furnace is 10~100MHz, and power is 200~1000w, temperature
It is 10~60min for room temperature~500 DEG C, reaction time.
Present invention also offers Manganese Based Cathode Materials for Lithium Ion Batteries prepared by any above-mentioned method.
Present invention also offers above-mentioned manganese-based anode material prepare lithium ion battery, motive-power battery, electric tool,
Application in medicine equipment and digital product.
Beneficial effects of the present invention
(1) the invention provides a kind of method for preparing manganese-based anode material, the method overcome in conventional preparation techniques
The ion mixing problem caused by aoxidizing insufficient doping with mechanical batch mixing, it is effectively improved the utilization rate of raw material so that production
The specific discharge capacity and multiplying power stability of product significantly improve, and are suitable for lithium-ion-power cell application field
(2) preparation method of the present invention is simple, cycle efficieny is high, practical, easy to spread.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
A kind of preparation method of lithium ion battery richness manganese anode material, it is characterised in that specifically include following steps：
(1) using manganese source, alkali lye and doped chemical as raw material, using preparation presoma containing manganese；
(2) then will contain manganese presoma and lithium salts ball milling mixing it is uniform after, be placed in plasma enhancing rotary furnace；
(3) oxygen-containing gas is passed through into above-mentioned rotary furnace by certain pressure and feed rate；
(4) frequency of setting plasma producing apparatus, power, voltage, temperature, reaction time；
(5) start plasma producing apparatus and prepare rich manganese anode material.
Manganese source compound in the step (1) is MnCl2、MnO2、MnSO4、Mn(NO3)2、(CH3COO)2Mn and MnC2O4
In one or more, described alkali lye be ammoniacal liquor, NaOH, KOH and Na2CO3In one or more, described doped chemical
For the one or more in Al, Se, Mg, Zn, Co, Ti, Ni, Fe, V, Cr, S, P.
Lithium salts described in the step (2) is Li2CO3、LiOH、CH3COOLi and Li2C2O4In one or more.
Pressure is 50~100pa in the step (3), and 0.01~10L/min of feed rate, oxygen-containing gas is oxygen-enriched sky
One or more in gas, purity oxygen and air.
Step (4) frequency is 20~100MHz, and power is 200~1000w, when temperature is room temperature~500 DEG C, reaction
Between be 10~60min.
Embodiment 1
Weigh a certain amount of Mn (NO3)2Add deionized water and be made into the mixed solution that concentration is 0.4 mol/L；Configuration
NaOH concentration is 0.4 mol/L, is successively inputted to belt stirrer respectively with flow pump and fills the anti-of a certain amount of deionized water
To answer in kettle, the temperature for controlling reaction solution in reactor is 50 DEG C, makes the pH=8 of reaction solution in reactor, stirring reaction 1 hour,
Discharging is carried out after the completion of reaction, is washed, is dried, heat treatment finally gives MnO2Presoma.
By mole 1:2 by Li2CO3、MnO2Presoma adds deionized water, and ball milling mixing uniformly, after drying is placed in full of oxygen
In the plasma rotary furnace (model OTF-1200X-S-II-4CV-PE) of gas, plasma revolution stove evacuation, make vacuum
Degree reaches below 100pa, and at the uniform velocity heating adds, and heating rate be 10 DEG C/min, when temperature reaches 500 DEG C, at beginning plasma
Manage (plasma treatment is synchronous with sintering process), processing time is 0.5 hour, the power of plasma is set as 150W, in stove
It is cold go after obtain LiMn2O4Material.It is spherical, average grain diameter 400nm to measure the product particle.LiMn2O4At room temperature
0.2C first discharge specific capacity is 125mAh/g, and capacity is still up to 120mAh/g after circulating 100 times.
Embodiment 2
It is 1 in molar ratio:3 weigh NiSO4And MnSO4, add deionized water be made into concentration be 0.2 mol/L solution with
The Na of 0.2 mol/L2CO3It is successively inputted to the reactor that belt stirrer fills a certain amount of deionized water respectively with flow pump
In, the temperature for controlling reaction solution in reactor is 50 DEG C, makes the pH=10 of reaction solution in reactor, stirring reaction 1 hour, through washing
Wash, dry, finally give Ni0.5Mn1.5(CO3)2Presoma.
By mole 1:2 by LiOH, Ni0.5Mn1.5(CO3)2Presoma uniformly, after drying is placed in deionized water ball milling mixing
In plasma rotary furnace (model OTF-1200X-S-II-4CV-PE) full of oxygen, plasma revolution stove evacuation,
Vacuum is set to reach below 100pa, at the uniform velocity heating adds, and heating rate is 10 DEG C/min, when temperature reaches 500 DEG C, starts
Ion processing (plasma treatment is synchronous with sintering process), processing time are 0.5 hour, set the power of plasma as
150W, in stove it is cold go after obtain LiNi0.5Mn1.5O4Material.It is spherical, average grain diameter 300nm to measure the product particle.
LiNi0.5Mn1.5O40.2C first discharge specific capacity is 130mAh/g at room temperature, and capacity is still reachable after circulating 100 times
125mAh/g。
Embodiment 3
By certain molar ratio weighing Mn (NO3)2、Co(NO3)2With Ni (NO3)2Addition deionized water is made into concentration and rubbed for 2
You/liter mixed solution；The concentration for configuring ammoniacal liquor is 2 mol/Ls, is successively inputted to belt stirrer respectively with flow pump and fills one
In the reactor of quantitative deionized water, the temperature for controlling reaction solution in reactor is 60 DEG C, makes the pH of reaction solution in reactor
=11, stirring reaction 1 hour, discharging is carried out after the completion of reaction, washed, dried, heat treatment finally gives Ni1/3Co1/3Mn1/3O2
Presoma.
By mole 1:2 by LiOH, Ni1/3Co1/3Mn1/3O2Presoma and deionized water ball milling mixing uniformly, after drying are placed in
In plasma reaction stove full of oxygen in (model OTF-1200X-S-II-4CV-PE), plasma rotary furnace is taken out very
Sky, vacuum is set to reach below 100pa, at the uniform velocity heating adds, and heating rate be 10 DEG C/min, when temperature reaches 300 DEG C, beginning
Plasma treatment (plasma treatment is synchronous with sintering process), processing time are 0.5 hour, set the power of plasma as
150W, in stove it is cold go after obtain LiNi1/3Co1/3Mn1/3O2Material.The product particle is measured to be spherical, average grain diameter is
150nm.Using lithium piece as negative pole, LiNi is measured1/3Co1/3Mn1/3O20.2C first discharge specific capacity is 145mAh/g at room temperature,
Capacity is still up to 140mAh/g after circulating 100 times.
Comparative example 1
By LiOH, Mn (NO3)2、Fe(NO3)3Uniformly, after drying the pipe full of argon gas is placed in deionized water ball milling mixing
In formula stove 850 DEG C handle 16 hours, in stove it is cold go after obtain LiMn1.5Fe0.5O4Material.The product particle is measured to be spherical,
Average grain diameter is 1um.LiMn1.5Fe0.5O40.2C first discharge specific capacity is 115mAh/g at room temperature, after circulating 100 times
Capacity is still up to 100mAh/g.
Comparative example 2
Li2CO3、MnO2、Ni(NO3)2Uniformly, after drying the plasma full of oxygen is placed in deionized water ball milling mixing
In reacting furnace 800 DEG C handle 12 hours, in stove it is cold go after obtain LiMn1.5Ni0.5O4Material.It is class ball to measure the product particle
Shape, average grain diameter 500nm.LiMn1.5Ni0.5O40.2C first discharge specific capacity is 121mAh/g at room temperature, circulation 100
Capacity is still up to 118mAh/g after secondary.
Finally it should be noted that the foregoing is only the preferred embodiments of the present invention, this hair is not limited to
Bright, although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it is still
Technical scheme described in previous embodiment can be modified, or equivalent substitution is carried out to which part.It is all in this hair
Within bright spirit and principle, any modification, equivalent substitution and improvements made etc., protection scope of the present invention should be included in
Within.Although the above-mentioned embodiment to the present invention is described, not limiting the scope of the invention, institute
Category art personnel should be understood that on the basis of technical scheme those skilled in the art need not pay wound
The various modifications or deformation that the property made work can be made are still within protection scope of the present invention.
Claims (10)
1. a kind of using plasma enhancing chemical vapor deposition (PECVD) technology prepares Manganese Based Cathode Materials for Lithium Ion Batteries
Method, it is characterised in that including：
The presoma containing manganese of co-electrodeposition method doping vario-property is well mixed with lithium salts, bar be present in the plasma of oxygen active particles
High-temperature process, cooling, produce manganese-based anode material under part.
2. the method as described in claim 1, it is characterised in that in the presoma containing manganese and lithium salts, Mn:Mole of Li elements
Than for 1：1.
3. the method as described in claim 1, it is characterised in that the preparation method of the presoma containing manganese is：With manganese source, alkali lye
It is raw material with doped chemical, prepared by co-electrodeposition method.
4. method as claimed in claim 3, it is characterised in that the manganese source compound is MnCl2、MnO2、MnSO4、Mn
(NO3)2、(CH3COO)2Mn and MnC2O4In one or more；
Described alkali lye is ammoniacal liquor, NaOH, KOH and Na2CO3In one or more；
Or the doped chemical is the one or more in Al, Se, Mg, Zn, Co, Ti, Ni, Fe, V, Cr, S, P.
5. the method as described in claim 1, it is characterised in that the lithium salts is Li2CO3、LiOH、CH3COOLi and Li2C2O4
In one or more.
6. the method as described in claim 1, it is characterised in that the pressure of the oxygen-containing gas is 50~100pa, feed rate
0.01~10L/min.
7. the method as described in claim 1, it is characterised in that the oxygen-containing gas is in oxygen-enriched air, purity oxygen and air
One or more.
8. the method as described in claim 1, it is characterised in that the frequency of the plasma enhancing rotary furnace be 20~
100MHz, power are 200~1000w, and temperature is room temperature~500 DEG C, the reaction time is 10~60min.
9. Manganese Based Cathode Materials for Lithium Ion Batteries prepared by the method described in claim any one of 1-8.
10. the manganese-based anode material described in claim 9 is preparing lithium ion battery, motive-power battery, electric tool, Medical treatment device
Application in tool and digital product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423650A (en) * | 2018-03-28 | 2018-08-21 | 山东省科学院能源研究所 | A kind of preparation method of lithium ion battery anode material lithium iron phosphate |
| CN111446445A (en) * | 2020-04-21 | 2020-07-24 | 西北工业大学 | Plasma treatment method for nickel-based lithium ion positive electrode material precursor |
| CN114551780A (en) * | 2022-01-27 | 2022-05-27 | 南京邮电大学 | Surface lithium-poor, sodium-poor or potassium-poor cathode material and plasma enhanced sintering method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106992296A (en) * | 2017-05-25 | 2017-07-28 | 宁波工程学院 | A kind of electromagnetic field containment plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
| CN107140696A (en) * | 2017-05-25 | 2017-09-08 | 宁波工程学院 | A kind of plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
-
2017
- 2017-10-31 CN CN201711043756.4A patent/CN107845807A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106992296A (en) * | 2017-05-25 | 2017-07-28 | 宁波工程学院 | A kind of electromagnetic field containment plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
| CN107140696A (en) * | 2017-05-25 | 2017-09-08 | 宁波工程学院 | A kind of plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423650A (en) * | 2018-03-28 | 2018-08-21 | 山东省科学院能源研究所 | A kind of preparation method of lithium ion battery anode material lithium iron phosphate |
| CN108423650B (en) * | 2018-03-28 | 2020-06-02 | 山东省科学院能源研究所 | Preparation method of lithium ion battery anode material lithium iron phosphate |
| CN111446445A (en) * | 2020-04-21 | 2020-07-24 | 西北工业大学 | Plasma treatment method for nickel-based lithium ion positive electrode material precursor |
| CN111446445B (en) * | 2020-04-21 | 2022-03-22 | 西北工业大学 | Plasma treatment method for nickel-based lithium ion positive electrode material precursor |
| CN114551780A (en) * | 2022-01-27 | 2022-05-27 | 南京邮电大学 | Surface lithium-poor, sodium-poor or potassium-poor cathode material and plasma enhanced sintering method and application thereof |
| CN114551780B (en) * | 2022-01-27 | 2023-11-24 | 南京邮电大学 | Positive electrode material with surface lean in lithium, lean in sodium or lean in potassium, and plasma enhanced sintering method and application thereof |
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Application publication date: 20180327 |