CN105036103A - Preparation method of cuboid lithium battery anode lithium ferric manganese phosphate material - Google Patents
Preparation method of cuboid lithium battery anode lithium ferric manganese phosphate material Download PDFInfo
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Abstract
The invention discloses a preparation method of a cuboid lithium battery anode lithium ferric manganese phosphate material. Precursor materials, namely, a Mn source compound, a Fe source compound, a P source compound and a Li source compound are weighed with the molar ratio of Mn to Fe to P to Li being 0.8:0.2:1:3 and are added with water to be dissolved; after an additive is dissolved, all the solutions are sequentially mixed and evenly stirred under argon protection; the PH value is regulated to 8-9 through ammonium hydroxide; the mixed system is transferred into a reaction still to be heated; obtained sediments are washed and subjected to centrifugal drying; finally, the sediments are mixed with an appropriate amount of carbon, and after grinding and calcining, the lithium ferric manganese phosphate material is obtained. The additive like a surface active agent or a complexing agent is added and jointed with generated microcrystal grain crystal nucleuses through ionic bonds or hydrogen bonds, the growth, in a certain direction, of grains is affected, the grains are made to grow in a specific direction, and therefore a product with a specific shape is formed.
Description
Technical field
The present invention relates to a kind of preparation method of anode material of lithium battery lithium ferric manganese phosphate, particularly a kind of preparation method of anode material of lithium battery lithium ferric manganese phosphate of rectangular parallelepiped pattern, belongs to energy technical field of new material preparation.
Background technology
In recent years, transition metal phosphate lithium salts LiMPO
4(M=Mn, Fe, Co, Ni) owing to having hypotoxicity, low cost, the chemical property of thermostability and great potential and attracted a lot of concerns.Compare and realize commercial LiFePO
4, (operating voltage 3.4V), LiMnPO
4should be more preferably LiCoO
2equivalent material, because its operating voltage (about 4.1V) is more close to LiCoO
2, also make it have to exceed than iron lithium phosphate the theoretical specific energy of 20%.But the native electronic specific conductivity that lithium manganese phosphate material is extremely low (is less than 10
-10s/cm, more than iron lithium phosphate also low 2 orders of magnitude, belongs to isolator), make it under quite little multiplying power, still only have extremely low specific storage, specific energy and cycle performance, limit its commercial applications.
The LiFe that current research is warmmer
xmn
1-xpO
4positive electrode material is exactly based on LiMnPO
4and LiFePO
4novel anode material between the two, the charge and discharge potential of this positive electrode material can be brought up to 4.1V (vs.Li) left and right by the introducing of Mn element, thus can improve the energy density of positive electrode material to a great extent.And by reasonably adjusting ferrimanganic ratio, and coated by carbon, the modified methods such as metal ion mixing, reduce Jahn-Teller effect, improve electronic conductivity and the ion transportation of material, thus obtain higher chemical property.At present for LiFe
xmn
1-xpO
4the research of the relation between the composition of material, structure and performance thereof is still less, traditional irregular uneven block materials, also exists that utilization ratio is low, lithium ion diffusion is slow, polarize the problem such as large, governs the lifting of lithium cell performance.The nano material with regular morphology has the structural advantage that reactive behavior is high, be conducive to charge-conduction and substance use and uniqueness, effectively can improve the performance of lithium cell.
High temperature solid-state method prepares LiFe at present
xmn
1-xpO
4one of method that positive electrode material is the most frequently used is the topmost a kind of powder preparation method adopted in suitability for industrialized production and scientific research at present.Although it is simple to have equipment and process, preparation condition easily controls, and easily realizes the advantage of industrialization.But energy consumption is high, the cycle is long, the shortcoming such as the chemical property of synthetic product is relatively poor, makes current researchist and enterprise all sight be turned to other preparation method advantageously.Hydrothermal method is a kind of simple, environmental protection, be easy to the synthetic method that regulates and controls, be widely used for synthesizing various material system, its principle accelerates ionic reaction and facilitation of hydrolysis reaction under hydrothermal condition, make the thermodynamical reaction that speed of reaction under some normal temperature and pressures is very slow, realize rapid reaction under hydrothermal conditions.The product of Hydrothermal Synthesis has good crystal habit, can by regulation and control reaction conditions, thus the shape of regulation and control product grain, good dispersity, the rule particle of uniform particle sizes contributes to lithium ion to carry out embedding and deviating from along a certain specific direction, thus improve the ionic conductivity of material, promote the chemical property of material.
In sum, solution method prepare lithium manganese phosphate material be one more promising, and method more with practical value, but how obtaining a kind of simply effective, convenient and swift and lower-cost method is an important research direction.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of simply effective, convenient and swift and preparation method of lower-cost cuboid-type anode material of lithium battery lithium ferric manganese phosphate.Use hydrothermal synthesis method, by adding the additive such as tensio-active agent or complexing agent, additive is linked together by the microcrystal grain nucleus of ionic linkage or hydrogen bond and generation, affects the growth of a direction of crystal grain, make it grow along specific direction, thus form the product of specific morphology.In addition, the electrostatic effect of additive and space steric effect can prevent particle from reuniting in the liquid phase, make powder keep good single dispersing.
In order to solve the problem, the present invention by the following technical solutions:
A kind of preparation method of cuboid-type lithium cell lithium ferric manganese phosphate positive electrode material, by persursor material manganese source compound, Fe source compound, P source compound and Li source compound, be 0.8:0.2:1:3 weighing by the mol ratio of Mn:Fe:P:Li element and be dissolved in water respectively, then after additive being dissolved, each solution is mixed successively, and stir under the condition passing into argon shield, pH value is regulated to be between 8 ~ 9 with ammoniacal liquor, mixed system is transferred in reactor and heats, the washing of precipitate centrifugal drying will obtained again, finally mix with appropriate carbon source, through grinding, calcination process, finally obtain lithium ferric manganese phosphate material.
Below the further optimization of the present invention to such scheme:
The method comprises the following steps:
A, take manganese source compound, Fe source compound, P source compound and Li source compound; by the mol ratio of Mn:Fe:P:Li element be 0.8:0.2:1:3 weigh; soluble in water respectively; form the manganese source of 1mol/L, source of iron solution, phosphorus source solution and Li source compound solution; under the condition passing into argon shield; manganese source and source of iron solution are mixed, then phosphorus source and Li source compound solution is added successively and stir.
B, by soluble in water for the additive of 0.5g, and to join in the mixing solutions of above-mentioned step A, and stir.
C, in whipping process, constantly pass into high-purity Ar or high pure nitrogen, to protect the Mn in solution
2+and Fe
2+not oxidized.The pH value of test soln, can be regulated between pH value scope 8 ~ 9 by ammoniacal liquor.
D, stir after, mixed system is transferred in reactor, and between 150 ~ 180 DEG C hydro-thermal reaction 8 ~ 12h, after having reacted, by precipitated product centrifuge washing, dry;
E, subsequently throw out and carbon source to be mixed; the amount of carbon source is that 1%-15% adds according to the content of carbon in final product; after grinding evenly; under the condition passing into protection of inert gas; first at 250 DEG C, 2h is calcined; then temperature is elevated between 600 DEG C ~ 800 DEG C, and calcining 4 ~ 12h, obtains the material of final product lithium ferric manganese phosphate carbon coated.
In such scheme, described additive be in cetyl trimethylammonium bromide, ethylenediamine tetraacetic acid (EDTA), polyvinylpyrrolidone wherein one or more.
Described manganese source is the one in manganous sulfate, manganous nitrate, manganous acetate, Manganous chloride tetrahydrate etc.
Described source of iron is the one in ferrous sulfate, ferrous ammonium sulphate, Iron nitrate, iron protochloride etc.
Described lithium source is the one in lithium hydroxide, lithium acetate, Lithium Sulphate, lithium nitrate etc.
Described phosphorus source to adopt in phosphoric acid, primary ammonium phosphate, Secondary ammonium phosphate wherein one or more.
Described carbon source adopts wherein one or more such as glucose, sucrose, starch, Mierocrystalline cellulose, pyrroles, fructose, acetylene black, SuperP, polystyrene.
Technique effect of the present invention is: adopt hydrothermal method preparation, obtain a kind of lithium ferric manganese phosphate material of cuboid-type, particle diameter is about between 50-500nm, and the structure of rectangular parallelepiped in charge and discharge process, can make Li
+along b direction of principal axis ordered movement, be conducive to the embedding of lithium ion and deviate from, thus improving Li
+the reaction kinetics of motion, improves ionic conductivity.Coated by second step carbon, obtain lithium ferric manganese phosphate carbon coated material after calcining, after carbon coated, improve the specific conductivity of material, enhance the conductivity of material.The material first discharge specific capacity obtained can reach more than 140mAh/g, and 1C specific discharge capacity can reach 130mAh/g, and 5C specific discharge capacity can reach more than 110mAh/g, shows good high rate performance.
Special rectangular structure serves very large active effect for the lifting of the final performance of material.
The present invention is by adding the additive such as tensio-active agent or complexing agent, additive is linked together by the microcrystal grain nucleus of ionic linkage or hydrogen bond and generation, affect the growth of a direction of crystal grain, make it grow along specific direction, thus form the product of specific morphology.In addition, the electrostatic effect of additive and space steric effect can prevent particle from reuniting in the liquid phase, make powder keep good single dispersing.Simply effective, convenient and swift and cost is lower.
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing explanation
Accompanying drawing 1 is product LiFe in the embodiment of the present invention 1
0.2mn
0.8pO
4the SEM figure of/C;
Accompanying drawing 2 is product LiFe in the embodiment of the present invention 2
0.2mn
0.8pO
4the SEM figure of/C;
Accompanying drawing 3 is product LiFe in the embodiment of the present invention 1
0.2mn
0.8pO
4the XRD figure of/C;
Accompanying drawing 4 is product LiFe in the embodiment of the present invention 1
0.2mn
0.8pO
4the 0.1C discharge curve first of/C;
Accompanying drawing 5 is product LiFe in the embodiment of the present invention 1
0.2mn
0.8pO
4the 1C cycle life graphic representation of/C;
Accompanying drawing 6 is product LiFe in the embodiment of the present invention 1
0.2mn
0.8pO
4the high rate performance graphic representation of/C.
Embodiment
Embodiment 1: a kind of preparation method of cuboid-type lithium cell lithium ferric manganese phosphate positive electrode material; comprise the following steps: the lithium acetate of 2.0402g is dissolved in 20ml water; the manganous sulfate of 2.7043g is dissolved in 20ml water; the ferrous ammonium sulphate of 1.5686g is joined in manganese sulfate solution; be stirred to dissolving; the process of dissolving and be uniformly mixed passes into protection of inert gas; by in the ammonium dihydrogen phosphate 20nl water of 2.3006g, lithium salt solution, phosphorus source solution and manganese source, source of iron mixing solutions are mixed.
The CTAB of 0.5g is dissolved in 15ml water, and adds the ethylene glycol of 5ml, then CTAB solution is joined in mixed system, regulate pH value to be 8.5 with ammoniacal liquor, mixing solutions is transferred in reactor, at 180 DEG C, react 8h, after having reacted, pelleting centrifugation is washed, dry, subsequently by intermediate product and the mixing of 0.6986g glucose, after grinding evenly, at high temperature calcine, first at 250 DEG C, 2h is calcined, then be elevated to 800 DEG C, calcining 4h, obtains lithium ferric manganese phosphate bag carbon material.
Accompanying drawing 1 is the SEM figure of the product that embodiment 1 obtains, and clearly, pattern is cuboid-type, and accompanying drawing 3 is for obtaining the XRD figure of product, and the diffraction peak obtained is consistent with the standard diagram of lithium ferric manganese phosphate, does not have impurity peaks to occur, illustrates that the product obtained is purer.
With the product obtained as positive electrode material, using metal lithium sheet as to electrode, use the barrier film of 32 μm, electrolytic solution employing solvent is the LiPF of the 1mol/L of EC, DMC, EMC
6electrolytic solution, in glove box, be assembled into CR2025 type button cell, adopt LANDCT2001A battery test system button type battery to carry out electric performance test, voltage range is 2.5 ~ 4.5V, current density is 1C=170mA/g, test result is as shown in accompanying drawing 4, accompanying drawing 5 and accompanying drawing 6, and 0.1C first discharge specific capacity reaches more than 140mAh/g, under 1C condition, after 80 circulations, specific storage can also reach more than 120mAh/g, even if multiplying power reaches 5C, specific storage is also at more than 110mAh/g.
Embodiment 2: a kind of preparation method of cuboid-type lithium cell lithium ferric manganese phosphate positive electrode material, comprises the following steps:
The lithium acetate of 2.0402g is dissolved in 20ml water; the manganous sulfate of 2.7043g is dissolved in 20ml water; the ferrous ammonium sulphate of 1.5686g is joined in manganese sulfate solution; be stirred to dissolving; the process of dissolving and be uniformly mixed passes into protection of inert gas; by in the ammonium dihydrogen phosphate 20nl water of 2.3006g, lithium salt solution, phosphorus source solution and manganese source, source of iron mixing solutions are mixed.The EDTA of 0.5g is dissolved in 15ml water, and adds the ethylene glycol of 5ml, then EDTA solution is joined in mixed system, regulate pH value to be 8.5 with ammoniacal liquor, mixing solutions is transferred in reactor, at 170 DEG C, react 10h, after having reacted, pelleting centrifugation is washed, dry, subsequently by intermediate product and the mixing of 0.6168g glucose, after grinding evenly, at high temperature calcine, first at 250 DEG C, 2h is calcined, then be elevated to 700 DEG C, calcining 8h, obtains lithium ferric manganese phosphate bag carbon material.
Accompanying drawing 2 is the SEM figure of the product that embodiment 2 obtains, and clearly, pattern is the cuboid-type of rule, and it is consistent that its XRD figure and embodiment 1 obtain, and the results are shown in accompanying drawing 3.
Embodiment 3: a kind of preparation method of cuboid-type lithium cell lithium ferric manganese phosphate positive electrode material, comprises the following steps:
The lithium acetate of 2.0402g is dissolved in 20ml water; the manganous sulfate of 2.7043g is dissolved in 20ml water; the ferrous ammonium sulphate of 1.5686g is joined in manganese sulfate solution; be stirred to dissolving; the process of dissolving and be uniformly mixed passes into protection of inert gas; by in the ammonium dihydrogen phosphate 20nl water of 2.3006g, lithium salt solution, phosphorus source solution and manganese source, source of iron mixing solutions are mixed.The CTAB of 0.5g is dissolved in 15ml water, and adds the ethylene glycol of 5ml, then CTAB solution is joined in mixed system, regulate pH value to be 8.5 with ammoniacal liquor, mixing solutions is transferred in reactor, at 150 DEG C, react 12h, after having reacted, pelleting centrifugation is washed, dry, subsequently by intermediate product and the mixing of 0.7504g glucose, after grinding evenly, at high temperature calcine, first at 250 DEG C, 2h is calcined, then be elevated to 600 DEG C, calcining 12h, obtains lithium ferric manganese phosphate bag carbon material.
Following table is the processing parameter in above-described embodiment:
Claims (11)
1. a preparation method for cuboid-type anode material of lithium battery lithium ferric manganese phosphate, is characterized in that:
By persursor material manganese source compound, Fe source compound, P source compound and Li source compound; be 0.8:0.2:1:3 weighing by Mn:Fe:P:Li elemental mole ratios and be dissolved in water respectively; then additive mixed dissolution is added; under the condition passing into protection of inert gas, each solution is mixed; carry out reacting by heating in a kettle.; finally mix with appropriate carbon source, grind successively, calcine, obtain product phosphoric acid ferrimanganic lithium bag carbon composite.
2. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, is characterized in that: the method comprises the following steps:
Be that 0.8:0.2:1:3 weighs by persursor material manganese source compound, Fe source compound, P source compound and Li source compound by Mn:Fe:P:Li elemental mole ratios, and the solution of respectively water-soluble formation 1mol/L;
By manganese source and source of iron mixing, phosphorus source and lithium source are mixed, the additive of 0.5g is dissolved in 20ml water, as tensio-active agent or complexing agent, additive solution is joined in the mixing solutions in ferromanganese source, and stir, then join in the mixed solution in phosphorus source and lithium source, and constantly stir;
Constantly pass into rare gas element, to protect the Mn in solution being uniformly mixed in process
2+and Fe
2+not oxidized;
The pH value of test soln, and regulated between pH value scope 8 ~ 9 by ammoniacal liquor.
3. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, is characterized in that: the method is further comprising the steps of:
After stirring, mixed system is transferred in reactor, and between 150 ~ 180 DEG C hydro-thermal reaction 8 ~ 12h, after having reacted, pelleting centrifugation is washed, dry; The precipitation obtained and carbon source are mixed, after grinding evenly, first at 250 DEG C, calcine 2h, be then elevated between 600 DEG C ~ 800 DEG C, calcining 4 ~ 12h, obtains product phosphoric acid ferrimanganic lithium bag carbon composite.
4. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described additive be in cetyl trimethylammonium bromide, ethylenediamine tetraacetic acid (EDTA), polyvinylpyrrolidone wherein one or more.
5. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described phosphorus source adopt in phosphoric acid, primary ammonium phosphate, Secondary ammonium phosphate wherein one or more, preferably phosphoric acid ammonium dihydrogen.
6. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described manganese source adopts the one in manganous sulfate, manganous nitrate, manganous acetate, Manganous chloride tetrahydrate etc.
7. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described source of iron is the one in ferrous sulfate, ferrous ammonium sulphate, Iron nitrate, iron protochloride etc.
8. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described lithium source is the one in lithium hydroxide, lithium acetate, Lithium Sulphate, lithium nitrate etc.
9. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1 and 2, is characterized in that: described carbon source adopts wherein one or more such as glucose, sucrose, starch, Mierocrystalline cellulose, pyrroles, fructose, acetylene black, SuperP, polystyrene.
10. the preparation method of a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 3, is characterized in that: the pH value ammoniacal liquor adjustable value 8 ~ 9 of described solution.
The preparation method of 11. a kind of cuboid-type anode material of lithium battery lithium ferric manganese phosphates according to claim 1, is characterized in that: described product is cuboid-type, and particle diameter is about between 50-500nm.
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| CN106450232A (en) * | 2016-11-30 | 2017-02-22 | 武汉理工力强能源有限公司 | Preparation method and application of novel lithium ion battery cathode material namely ternary phosphate |
| CN107720719A (en) * | 2017-11-03 | 2018-02-23 | 山东科技大学 | The method for preparing iron manganese phosphate for lithium using siderite and manganese spar |
| CN108493449A (en) * | 2018-03-20 | 2018-09-04 | 苏州大学 | A kind of method of controllable preparation manganese fluorophosphate sodium positive electrode |
| CN108539161A (en) * | 2018-04-04 | 2018-09-14 | 广州大学 | A kind of olive-type lithium manganese phosphate preparation method of the surface with prismatic protrusion |
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| CN108493449A (en) * | 2018-03-20 | 2018-09-04 | 苏州大学 | A kind of method of controllable preparation manganese fluorophosphate sodium positive electrode |
| CN108539161A (en) * | 2018-04-04 | 2018-09-14 | 广州大学 | A kind of olive-type lithium manganese phosphate preparation method of the surface with prismatic protrusion |
| CN108539161B (en) * | 2018-04-04 | 2020-12-01 | 广州大学 | Preparation method of olive-shaped lithium manganese phosphate with prismatic protrusions on surface |
| CN109103452A (en) * | 2018-08-28 | 2018-12-28 | 重庆大学 | The preparation method of nano lithium iron manganese anode composite material |
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| CN114497540A (en) * | 2022-01-26 | 2022-05-13 | 湖南裕能新能源电池材料股份有限公司 | Embedded lithium ferric manganese phosphate cathode material, preparation method thereof, lithium ion battery and electric equipment |
| CN114497540B (en) * | 2022-01-26 | 2024-05-14 | 湖南裕能新能源电池材料股份有限公司 | Embedded lithium iron manganese phosphate positive electrode material, preparation method thereof, lithium ion battery and electric equipment |
| CN114644329A (en) * | 2022-04-12 | 2022-06-21 | 深圳沃伦特新能源科技有限公司 | Hydrothermal synthesis method of nano lithium ferric manganese phosphate |
| CN116081589A (en) * | 2022-10-12 | 2023-05-09 | 北京钠谛科技有限公司 | Lithium-rich lithium iron manganese phosphate material and preparation method thereof |
| CN116081589B (en) * | 2022-10-12 | 2024-03-29 | 北京钠谛科技有限公司 | Lithium-rich lithium iron manganese phosphate material and preparation method thereof |
| CN116374987A (en) * | 2023-04-12 | 2023-07-04 | 安徽洁途新能源科技有限公司 | Preparation method of lithium iron manganese phosphate |
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