CN102290564A - Positive electrode material of secondary battery and preparation method thereof - Google Patents
Positive electrode material of secondary battery and preparation method thereof Download PDFInfo
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- CN102290564A CN102290564A CN2011101938400A CN201110193840A CN102290564A CN 102290564 A CN102290564 A CN 102290564A CN 2011101938400 A CN2011101938400 A CN 2011101938400A CN 201110193840 A CN201110193840 A CN 201110193840A CN 102290564 A CN102290564 A CN 102290564A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a positive electrode material of a secondary battery. The method comprises the following steps: mixing a vanadium source compound with an organic solvent to obtain a vanadium source compound solution; adding LiMn2O4 into the vanadium source compound solution, standing and then drying, thus obtaining a first mixture; and warming the first mixture in oxygen-containing gas, performing heat preservation, and reacting to obtain the lithium manganate positive electrode material coated with vanadic oxide. Compared with the prior art, the preparation method has the advantages that after the vanadium source compound solution is prepared, the vanadium source compound is uniformly dispersed at the surface of a LiMn2O4 material by use of a soaking method and then the vanadium source compound reacts with oxygen gas by virtue of a heating step, thus the lithium manganate positive electrode material coated with vanadic oxide is prepared, therefore the operation is simple, and a ball milling method is not required, thereby achieving less energy consumption and being beneficial to industrialized production. Experimental results indicate that the positive electrode material prepared by the invention has the advantages of favorable cycle performance and high-temperature stability.
Description
Technical field
The present invention relates to the battery technology field, more particularly, relate to positive electrode of a kind of secondary cell and preparation method thereof.
Background technology
In recent years, along with highlighting of the problems such as exhausted day by day and global warming of resource, the life style of green low-carbon has been subjected to advocating.The research and development of electric motor car and hybrid electric vehicle can partly replace the internal-combustion engines vehicle of consumption of fossil fuels, is one of main method that solves energy crisis and ecological deterioration.Driving power is to influence the critical component that electric motor car is promoted the use of, and nowadays widely used driving power comprises lead-acid battery, secondary cells such as ni-mh/NI-G, lithium ion battery.Secondary cell is meant, can make active material activate the battery that continues use by the mode of charging behind battery discharge.Advantages such as in various secondary cells, lithium ion battery is owing to have the energy density height, and cyclicity is good, and self-discharge rate is low, long service life and environmental pressure are little have obtained extensive studies.
The positive electrode that uses in the lithium ion battery comprises lithium cobaltate cathode material, manganate cathode material for lithium etc.For lithium cobaltate cathode material, because the abundance of cobalt element in the earth's crust is low, thereby price is higher, in addition, cobalt element also has certain toxicity, and discarded back is bigger to environmental hazard, so there are problems such as cost height, discarded after stain environment, security performance be relatively poor in lithium cobaltate cathode material.Compare with manganate cathode material for lithium, manganate cathode material for lithium have aboundresources, cheap, fail safe good, voltage platform is high, nontoxic pollution-free and be easy to characteristics such as preparation.But manganate cathode material for lithium exists cycle performance relatively poor, especially under hot conditions (55 ℃), there is serious capacity attenuation problem in it, cause battery performance to descend, therefore, the cycle performance and the high temperature stability performance that improve manganate cathode material for lithium are the focuses of current research.
At present, the common method of improving manganate cathode material for lithium cycle performance and high-temperature stability is doping method and method for coating etc.For example, application number is that 201010505801.5 Chinese patent literature has been reported a kind of lithium manganate having spinel structure electrode material and preparation method thereof, and this method adopts ball grinding method with Al
2O
3Be coated on LiMn
2O
4The surface, may further comprise the steps: preparation modification manganate precursor for lithium, do mixed, once sintered, ball milling coating and double sintering.But, above-mentioned reported method complicated operation, power consumption is big, is unsuitable for suitability for industrialized production.
Summary of the invention
In view of this, positive electrode that provides by a kind of secondary cell and preparation method thereof is provided the technical problem to be solved in the present invention, this method is simple to operate, and it is less to consume energy, and the manganate cathode material for lithium that the vanadic oxide for preparing coats has excellent cycle performance and high temperature stability performance.
The invention provides a kind of preparation method of positive electrode of secondary cell, may further comprise the steps:
The vanadium source compound is mixed with organic solvent, obtain vanadium source compound solution, described vanadium source compound is that vanadium acetylacetonate, praseodynium close vanadium and/or an oxygen two (oxalate) closes ammonium vanadate;
In described vanadium source compound solution, add LiMn
2O
4, leave standstill the back drying, obtain first mixture;
Described first mixture is warming up to 450～600 ℃ and insulation in oxygen-containing gas, obtains the manganate cathode material for lithium that vanadic oxide coats after the reaction.
Preferably, described organic solvent is ethanol, ether, chloroform or acetone.
Preferably, described LiMn
2O
4With the mass volume ratio of described vanadium source compound solution be 1g: (1～6) mL.
Preferably, described vanadium source compound and described LiMn
2O
4Mass ratio be (0.5～15): 100.
Preferably, described time of repose is 0.5～24 hour.
Preferably, described heating rate is 5～10 ℃/min.
Preferably, described intensification temperature is 500～550 ℃.
Preferably, described temperature retention time is 0.5～8 hour.
Preferably, described LiMn
2O
4Preparation as follows:
Lithium acetate, manganese acetate, citric acid and ammoniacal liquor are mixed, obtain second mixture after the drying;
Described second mixture 350 ℃～800 ℃ following calcinations, is obtained LiMn after the reaction
2O
4
Accordingly, the present invention also provides a kind of positive electrode of secondary cell of technique scheme preparation.
The invention provides a kind of preparation method of positive electrode of secondary cell, may further comprise the steps: the vanadium source compound is mixed with organic solvent, obtain vanadium source compound solution; In described vanadium source compound solution, add LiMn
2O
4, leave standstill the back drying, obtain first mixture; Described first mixture is heated up in oxygen-containing gas and be incubated, obtain the manganate cathode material for lithium that vanadic oxide coats after the reaction.Compared with prior art, the present invention adopts infusion method that the vanadium source compound is dispersed in LiMn behind preparation vanadium source compound solution
2O
4Material surface, then by heating steps with vanadium source compound and oxygen reaction, thereby prepare the manganate cathode material for lithium that vanadic oxide coats.Therefore, the present invention is simple to operate, need not to adopt ball grinding method, thereby it is less to consume energy, and helps suitability for industrialized production.Experimental result shows that the positive electrode that the present invention prepares has excellent cycle performance and high temperature stability performance.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the LiMn of the embodiment of the invention 1 preparation
2O
4/ V
2O
5The XRD figure spectrum of positive electrode;
Fig. 2 is the LiMn of the embodiment of the invention 1 preparation
2O
4/ V
2O
5The ESEM picture of positive electrode;
Fig. 3 is the LiMn of the embodiment of the invention 1 preparation
2O
4/ V
2O
5The XPS collection of illustrative plates of positive electrode;
Fig. 4 is that the lithium ion battery of the embodiment of the invention 4 and embodiment 7 preparations is at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C multiplying power and the relation curve of cycle period;
Fig. 5 is that the lithium ion battery of the embodiment of the invention 4 and embodiment 7 preparations is at the specific discharge capacity of 1C, 2C multiplying power and the relation curve of cycle period.
Embodiment
Below the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that is obtained under the creative work prerequisite.
The invention discloses a kind of preparation method of positive electrode of secondary cell, may further comprise the steps:
The vanadium source compound is mixed with organic solvent, obtain vanadium source compound solution, described vanadium source compound is that vanadium acetylacetonate, praseodynium close vanadium and/or an oxygen two (oxalate) closes ammonium vanadate;
In described vanadium source compound solution, add LiMn
2O
4, leave standstill the back drying, obtain first mixture;
Described first mixture is warming up to 450～600 ℃ and insulation in oxygen-containing gas, obtains the manganate cathode material for lithium that vanadic oxide coats after the reaction.
In the present invention, described organic solvent is preferably ethanol, ether, chloroform or acetone, more preferably ethanol.The vanadium source compound that the present invention adopts can dissolve in described organic solvent, and described vanadium source compound is preferably vanadium acetylacetonate.There is no particular restriction to the mass concentration of described vanadium source compound solution in the present invention, is preferably 0.5wt%～5wt%, and more preferably 1wt%～3wt% most preferably is 1.5wt%～2.5wt%.
After preparing vanadium source compound solution, in described vanadium source compound solution, add LiMn
2O
4, described LiMn
2O
4Be preferably 1g with the mass volume ratio of described vanadium source compound solution: (1～6) mL, more preferably 1g: (1～3) mL most preferably is 1g: (1.5～2.5) mL.In the present invention, above-mentioned preferred mass volume ratio can make just submergence LiMn of vanadium source compound solution
2O
4, LiMn
2O
4With the excessive or too small vanadium source compound that all can make of the mass volume ratio of described vanadium source compound solution at LiMn
2O
4Material surface disperses inhomogeneous, in addition, and LiMn
2O
4Cross low meeting with the mass volume ratio of described vanadium source compound solution and increase cost.
Among the present invention, described vanadium source compound and described LiMn
2O
4Mass ratio be preferably (0.5～15): 100, more preferably (1～10): 100, most preferably be (2～10): 100.In the step that obtains first mixture, described time of repose is preferably 0.5～24 hour, more preferably 1～20 hour, most preferably is 1～5 hour.Wherein, the method for described drying can be air dry, also can dry under the condition of 100 ℃ of heating, and to this, there is no particular restriction in the present invention.
Described LiMn
2O
4Can adopt method preparation well known to those skilled in the art, preferably be prepared as follows: lithium acetate, manganese acetate, citric acid and ammoniacal liquor are mixed, obtain second mixture after the drying; Described second mixture 350 ℃～800 ℃ following calcinations, is obtained LiMn after the reaction
2O
4Wherein, described the step of second mixture 350 ℃～800 ℃ of following calcinations is specially: described second mixture 350 ℃ of following calcinations 4～6 hours, is warming up to 800 ℃ of calcinations 8～12 hours then.
According to the present invention, in the step of the manganate cathode material for lithium that obtains the vanadic oxide coating, described temperature retention time is preferably 0.5～8 hour, more preferably 1～6 hour, most preferably be 1～4 hour, described heating rate is preferably 5～10 ℃/min, and more preferably 6～9 ℃/min most preferably is 7～8 ℃/min; Described intensification temperature is preferably 500～550 ℃, more preferably 500～530 ℃.Described intensification temperature is crossed when hanging down, and the decomposing oxidation time of vanadium source compound will rise appreciably; When this temperature is too high, LiMn
2O
4Be prone to the phenomenon of gathering, therefore, the preferred temperature and time that the present invention adopts can guarantee at LiMn
2O
4The surface generates the pentoxide layer of uniformity.With the vanadium source compound is that vanadium acetylacetonate is an example, its in air, 500 ℃ following reactions take place down:
4(C
5H
7O
2)
2VO+29O
2→2V
2O
5+20CO
2+28H
2O
The present invention adopts infusion method that the vanadium source compound is dispersed in LiMn
2O
4Material surface, then by heating steps with vanadium source compound and oxygen reaction, prepare the manganate cathode material for lithium that vanadic oxide coats.Therefore, preparation method provided by the invention is simple to operate, need not to adopt the method for ball milling, has avoided the energy consumption issues that adopts ball-milling method to produce, and helps suitability for industrialized production.In addition, because vanadic oxide has higher initial specific capacity, better cycle performance and high-temperature stability, therefore, with LiMn
2O
4Material is compared, and the manganate cathode material for lithium that the vanadic oxide of the present invention preparation coats has excellent cycle performance and high-temperature stability, and has guaranteed that the initial specific capacity of positive electrode of preparation is higher.
In order to further specify technical scheme of the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
Embodiment 1
It is soluble in water to be in the mol ratio of Li: Mn that 1: 2 ratio takes by weighing behind lithium acetate and the manganese acetate, adds aqueous citric acid solution then, regulates pH to 6.4 with ammoniacal liquor, obtains precipitation; Described sedimentation and filtration, dry back were burnt 5 hours at the beginning of under 350 ℃, be warming up to 800 ℃ of calcinations 10 hours then, obtain LiMn with the stove cooling
2O
4
Get 2.0g LiMn
2O
4Place the ethanolic solution of the vanadium acetylacetonate of 4mL 7.28wt%, soak after 2 hours 100 ℃ dry down, place Muffle furnace to be warming up to 500 ℃ and keep after 4 hours obtaining LiMn then with the stove cooling with the speed of 10 ℃/min
2O
4/ V
2O
5Positive electrode.
As shown in Figure 1, the LiMn for preparing for present embodiment
2O
4/ V
2O
5The XRD figure spectrum of positive electrode, as can be seen from the figure, LiMn
2O
4/ V
2O
5The crystal structure of positive electrode is LiMn
2O
4Spinel-type; Fig. 2 is the LiMn of present embodiment preparation
2O
4/ V
2O
5The ESEM picture of positive electrode, as can be seen from the figure, this LiMn
2O
4/ V
2O
5Positive electrode is 300～500nm particle; Fig. 3 is the LiMn of preparation
2O
4/ V
2O
5The XPS spectrum figure of positive electrode as can be seen from the figure, has the spectrum peak to belong to V at the 517.15eV place
2p
3/2V
2O
5The characteristic spectrum peak, shown that there is V on the positive electrode surface of present embodiment preparation
2O
5Exist.
It is soluble in water to be in the mol ratio of Li: Mn that 1: 2 ratio takes by weighing behind lithium acetate and the manganese acetate, adds aqueous citric acid solution then, regulates pH to 6.4 with ammoniacal liquor, obtains precipitation; With described sedimentation and filtration, burnt 5 hours at the beginning of under 350 ℃ dry back, is warming up to 800 ℃ of calcinations 10 hours then, with the stove cooling, obtains LiMn
2O
4
Get 2.0g LiMn
2O
4Place the ethanolic solution of 4mL 3.64wt% vanadium acetylacetonate, soak after 2 hours 100 ℃ dry down, place Muffle furnace to be warming up to 500 ℃ and keep after 4 hours obtaining LiMn then with the stove cooling with the speed of 10 ℃/min
2O
4/ V
2O
5Positive electrode.
Embodiment 3
It is soluble in water to be in the mol ratio of Li: Mn that 1: 2 ratio takes by weighing behind lithium acetate and the manganese acetate, adds aqueous citric acid solution then, regulates pH to 6.4 with ammoniacal liquor, obtains precipitation; With described sedimentation and filtration, burnt 5 hours at the beginning of under 350 ℃ dry back, is warming up to 800 ℃ of calcinations 10 hours then, with the stove cooling, obtains LiMn
2O
4
Get 2.0g LiMn
2O
4Place the ethanolic solution of 4mL 14.56wt% vanadium acetylacetonate, soak after 30 hours 100 ℃ dry down, place Muffle furnace to be warming up to 500 ℃ and keep after 4 hours obtaining LiMn then with the stove cooling with the speed of 10 ℃/min
2O
4/ V
2O
5Positive electrode.
Comparative example
It is soluble in water to be in the mol ratio of Li: Mn that 1: 2 ratio takes by weighing behind lithium acetate and the manganese acetate, adds aqueous citric acid solution then, regulates pH to 6.4 with ammoniacal liquor, obtains precipitation; With described sedimentation and filtration, burnt 5 hours at the beginning of under 350 ℃ the drying back, is warming up to 800 ℃ of calcinations 10 hours then, with the stove cooling, gets LiMn
2O
4
With described LiMn
2O
4Be warming up to 500 ℃ and kept 4 hours with the speed of 10 ℃/min,, obtain LiMn with the stove cooling
2O
4Positive electrode.
Positive electrode and conductive black Super P, N-methyl pyrrolidone (PVDF) with embodiment 1～3 and comparative example preparation mixes by mass ratio at 8: 1: 1 respectively, coat on the aluminium foil uniformly with rubbing method, place vacuum drying chamber 120 ℃ of dryings 12 hours then, move to then in the glove box that is full of high-purity argon gas, with LiPF
6Be the supporting electrolyte in the electrolyte, solvent is that volume ratio is 1: 1 EC and DEC, is the imbibition film with the glass fiber filter paper, and the PP film is a barrier film, makes CR2016 type button lithium ion battery.
Charge-discharge performance at the lithium ion battery of 55 ℃ of following test implementation examples, 4～7 preparations.Fig. 4 is that the lithium ion battery of embodiment 4 and embodiment 7 preparations is at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C multiplying power and the relation curve of cycle period, as can be seen from the figure, the lithium ion battery of embodiment 4 preparations is respectively 121.1 at the specific discharge capacity of 0.2C, 0.5C, 1C and 2C, 108.4,96.9 and 79.0mAh/g.Discharge and recharge 5 all after dates under the lithium ion battery 0.2C multiplying power with embodiment 4 and embodiment 7 preparations and under identical multiplying power, discharge and recharge again, obtain embodiment 4 and embodiment 7 preparations as shown in Figure 5 lithium ion battery at the specific discharge capacity of 1C, 2C multiplying power and the relation curve of cycle period.As shown in Figure 5, the lithium ion battery of embodiment 4 preparation first specific discharge capacity under 1C and 2C multiplying power is respectively 106.5mAh/g and 70.3mAh/g, is respectively 77.28% and 81.65% at the capability retention of circulation 200 all after dates.
In embodiment 5 and embodiment 6, adopt said method that the chemical property of the positive electrode of embodiment 2, embodiment 3 preparations is measured respectively, the lithium ion battery that obtains following result: embodiment 5 preparation first specific discharge capacity under 1C and 2C multiplying power is respectively 109.5mAh/g and 78.3mAh/g, is respectively 75.07% and 80.20% at the capability retention of circulation 200 all after dates.The lithium ion battery of embodiment 6 preparation first specific discharge capacity under the 1C multiplying power is 102.3mAh/g, is 82.40% at the capability retention of circulation 200 all after dates.
Embodiment 7 adopts said method that the chemical property of the positive electrode of comparative example preparation is measured, the lithium ion battery that obtains following result: embodiment 7 preparations is respectively 111.3mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C and 2C, 96.9mAh/g, 50.8mAh/g and 13.2mAh/g, first specific discharge capacity is respectively 38.8mAh/g and 23.6mAh/g under 1C and 2C multiplying power, is respectively 66.75% and 88.98% at the capability retention of circulation 200 all after dates.
Can show that from The above results the manganate cathode material for lithium that the vanadic oxide of the present invention's preparation coats has excellent cycle performance and high temperature stability performance.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined herein General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. the preparation method of the positive electrode of a secondary cell may further comprise the steps:
The vanadium source compound is mixed with organic solvent, obtain vanadium source compound solution, described vanadium source compound is that vanadium acetylacetonate, praseodynium close vanadium and/or an oxygen two (oxalate) closes ammonium vanadate;
In described vanadium source compound solution, add LiMn
2O
4, leave standstill the back drying, obtain first mixture;
Described first mixture is warming up to 450～600 ℃ and insulation in oxygen-containing gas, obtains the manganate cathode material for lithium that vanadic oxide coats after the reaction.
2. preparation method according to claim 1 is characterized in that, described organic solvent is ethanol, ether, chloroform or acetone.
3. preparation method according to claim 1 is characterized in that, described LiMn
2O
4With the mass volume ratio of described vanadium source compound solution be 1g: (1～6) mL.
4. preparation method according to claim 1 is characterized in that, described vanadium source compound and described LiMn
2O
4Mass ratio be (0.5～15): 100.
5. preparation method according to claim 1 is characterized in that, described time of repose is 0.5～24 hour.
6. preparation method according to claim 1 is characterized in that, described heating rate is 5～10 ℃/min.
7. preparation method according to claim 1 is characterized in that, described intensification temperature is 500～550 ℃.
8. preparation method according to claim 1 is characterized in that, described temperature retention time is 0.5～8 hour.
9. preparation method according to claim 1 is characterized in that, described LiMn
2O
4Preparation as follows:
Lithium acetate, manganese acetate, citric acid and ammoniacal liquor are mixed, obtain second mixture after the drying;
Described second mixture 350 ℃～800 ℃ following calcinations, is obtained LiMn after the reaction
2O
4
10. the positive electrode of the secondary cell of any preparation of claim 1～9.
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637871A (en) * | 2012-04-19 | 2012-08-15 | 中南大学 | Preparation method of lithium ion anode material coated with lithium ion activating oxide V2O5 |
| CN103187563A (en) * | 2011-12-27 | 2013-07-03 | 比亚迪股份有限公司 | Anode material for lithium-ion battery, preparation method for same, and lithium-ion battery |
| CN107732246A (en) * | 2017-10-30 | 2018-02-23 | 中南大学 | A kind of method of modifying of anode material for lithium-ion batteries solution dipping cladding |
| CN109888268A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A kind of lithium primary battery oxide/fluorination carbon composite anode material and preparation method thereof |
| CN110085854A (en) * | 2019-06-05 | 2019-08-02 | 骆驼集团武汉光谷研发中心有限公司 | A kind of vanadium phosphate cathode material and preparation method thereof |
| CN110676450A (en) * | 2019-10-16 | 2020-01-10 | 南昌工程学院 | Secondary battery anode material and battery thereof |
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| CN1627550A (en) * | 2003-12-11 | 2005-06-15 | 比亚迪股份有限公司 | Anode material of lithium ion cell and preparation method |
| CN1787254A (en) * | 2004-12-09 | 2006-06-14 | 比亚迪股份有限公司 | Lithium ion cell positive electrode actived material and preparation method thereof |
| CN101481145A (en) * | 2008-01-12 | 2009-07-15 | 鲁东大学 | Novel method for preparing lithium ionic cell anode material LiMn2O4 |
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| WO2004010519A1 (en) * | 2002-07-23 | 2004-01-29 | Nikko Materials Co., Ltd. | Method for producing positive plate material for lithium secondary cell |
| CN1627550A (en) * | 2003-12-11 | 2005-06-15 | 比亚迪股份有限公司 | Anode material of lithium ion cell and preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103187563A (en) * | 2011-12-27 | 2013-07-03 | 比亚迪股份有限公司 | Anode material for lithium-ion battery, preparation method for same, and lithium-ion battery |
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| CN102637871A (en) * | 2012-04-19 | 2012-08-15 | 中南大学 | Preparation method of lithium ion anode material coated with lithium ion activating oxide V2O5 |
| CN107732246A (en) * | 2017-10-30 | 2018-02-23 | 中南大学 | A kind of method of modifying of anode material for lithium-ion batteries solution dipping cladding |
| CN109888268A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A kind of lithium primary battery oxide/fluorination carbon composite anode material and preparation method thereof |
| CN109888268B (en) * | 2017-12-06 | 2023-12-01 | 中国科学院大连化学物理研究所 | Oxide/fluorocarbon composite positive electrode material for lithium primary battery and preparation method thereof |
| CN110085854A (en) * | 2019-06-05 | 2019-08-02 | 骆驼集团武汉光谷研发中心有限公司 | A kind of vanadium phosphate cathode material and preparation method thereof |
| CN110676450A (en) * | 2019-10-16 | 2020-01-10 | 南昌工程学院 | Secondary battery anode material and battery thereof |
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Application publication date: 20111221 |