CN105036103B - A kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate - Google Patents

A kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate Download PDF

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CN105036103B
CN105036103B CN201510481004.0A CN201510481004A CN105036103B CN 105036103 B CN105036103 B CN 105036103B CN 201510481004 A CN201510481004 A CN 201510481004A CN 105036103 B CN105036103 B CN 105036103B
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lithium
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cuboid
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CN105036103A (en
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王瑗钟
熊俊威
王盈盈
张建新
马春响
李魁忠
张风太
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Shandong Wina Green Power Technology Co Ltd
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Abstract

The invention discloses a kind of preparation method of cuboid-type lithium battery lithium ferric manganese phosphate positive electrode, by persursor material manganese source compound, Fe source compound, P source compound and Li source compound, by Mn:Fe:P:The mol ratio of Li elements is 0.8:0.2:1:3 weigh and are dissolved in water respectively, then after additive is dissolved, each solution is mixed successively, and stirred under conditions of argon gas protection is passed through, with ammoniacal liquor regulation pH value be 8 ~ 9 between, mixed system is transferred in reactor and heated, again by obtained washing of precipitate centrifugal drying, finally mixed with appropriate carbon source, by grinding, calcination process, finally give lithium ferric manganese phosphate material, the present invention is by adding the additives such as surfactant or complexing agent, additive is linked together by ionic bond or hydrogen bond and the microcrystal grain nucleus of generation, influence the growth of a direction of crystal grain, it is set to be grown along specific direction, so as to form the product of specific morphology.

Description

A kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate
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 cuboid pattern Anode material of lithium battery lithium ferric manganese phosphate preparation method, belong to energy technical field of new material preparation.
Background technology
In recent years, transition metal phosphate lithium salts LiMPO4(M=Mn, Fe, Co, Ni)Due to hypotoxicity, low cost, heat The chemical property of stability and great potential and attracted many concerns.Compared to the LiFePO for having realized commercialization4, (work Make voltage 3.4V), LiMnPO4Should be more preferably LiCoO2Alternative materials, because of its operating voltage(About 4.1V)It is more nearly LiCoO2, also make its possess be higher by than LiFePO4 20% theoretical specific energy.However, the extremely low intrinsic electricity of lithium manganese phosphate material Electron conductivity(Less than 10-10More than s/cm, 2 orders of magnitude also lower than LiFePO4, belong to insulator), make it fairly small Still there was only extremely low specific capacity, specific energy and cycle performance under multiplying power, limit its commercial applications.
The hotter LiFe of current researchxMn1-xPO4Positive electrode, is namely based on LiMnPO4And LiFePO4Between the two Novel anode material, the introducing of Mn elements can bring up to the charge and discharge potential of the positive electrode 4.1V (vs. Li) left and right, So as to largely improve the energy density of positive electrode.And by reasonably adjusting ferrimanganic ratio, and pass through carbon bag Cover, the modified method such as metal ion mixing, reduce Jahn-Teller effects, improve electronic conductivity and the ion transmission of material Speed, so as to obtain higher chemical property.At present for LiFexMn1-xPO4Between composition, structure and its performance of material Relation still less, the traditional irregular uneven block materials of research, exist that utilization rate is low, lithium ion diffusion Slowly the problems such as, polarizing big, governs the lifting of lithium battery performance.Nano material with regular morphology have reactivity it is high, Be conducive to charge-conduction and material to convey and unique structural advantage, the performance of lithium battery can be effectively improved.
High temperature solid-state method is current preparation LiFexMn1-xPO4One of positive electrode most common method, is at present in industry Metaplasia is produced and the topmost a kind of powder preparation method used in scientific research.Although simple with equipment and technique, preparation condition It is easily controlled, easily realizes the advantage of industrialization.But high energy consumption, cycle are long, the chemical property of synthetic product is relatively poor The shortcomings of so that sight is all turned to other preparation methods advantageously by current researcher and enterprise.Hydro-thermal method is A kind of synthetic method that is simple and environmentally-friendly, being easy to regulation and control, is widely used for synthesizing various material systems, its principle is hydro-thermal Under the conditions of accelerate ionic reaction and promote hydrolysis, make the very slow thermodynamical reaction of reaction rate under some normal temperature and pressures, Rapid reaction is realized under hydrothermal condition.The product of Hydrothermal Synthesiss has preferable crystal habit, can be by regulating and controlling reaction bar Part, so as to regulate and control the shape of product grain, good dispersion, the rule particle of uniform particle sizes contributes to lithium ion along a certain specific Direction be embedded in and deviate from, so as to improve the ionic conductivity of material, lift the chemical property of material.
In summary, it is that a comparison is promising that solwution method, which prepares lithium manganese phosphate material, and side relatively more with practical value Method, still, how to obtain a kind of easy and effective, convenient and swift and lower-cost method is an important research direction.
The content of the invention
The problem to be solved in the present invention is to provide a kind of easy and effective, convenient and swift and lower-cost cuboid-type lithium The preparation method of battery positive pole material phosphoric acid ferrimanganic lithium.With hydrothermal synthesis method, by adding surfactant or complexing agent Deng additive, additive is linked together by the microcrystal grain nucleus of ionic bond or hydrogen bond and generation, influences a certain of crystal grain The growth in direction, makes it be grown along specific direction, so as to form the product of specific morphology.In addition, the electrostatic effect of additive It can prevent particle from reuniting in the liquid phase with space steric effect, powder is kept preferable single dispersing.
In order to solve the above problems, the present invention uses following technical scheme:
A kind of preparation method of cuboid-type lithium battery lithium ferric manganese phosphate positive electrode, by persursor material manganese source chemical combination Thing, Fe source compound, P source compound and Li source compound, by Mn:Fe:P:The mol ratio of Li elements is 0.8:0.2:1:3 claim Measure and be dissolved in water respectively, after then additive is dissolved, each solution is mixed successively, and in the condition for being passed through argon gas protection Under stir, be between 8 ~ 9, mixed system to be transferred in reactor and heated with ammoniacal liquor regulation pH value, then heavy by what is obtained Form sediment washing centrifugal drying, is finally mixed with appropriate carbon source, by grinding, calcination process, finally gives lithium ferric manganese phosphate material.
Further optimization the following is the present invention to such scheme:
This method comprises the following steps:
A, manganese source compound, Fe source compound, P source compound and Li source compound are weighed, by Mn:Fe:P:Li elements Mol ratio is 0.8:0.2:1:3 weigh, soluble in water respectively, form 1mol/L manganese source, source of iron solution, phosphorus source solution and lithium source Compound solution, under conditions of argon gas protection is passed through, manganese source and source of iron solution is well mixed, then by phosphorus source and lithium source Polymer solution is sequentially added and stirred.
It is B, 0.5g additive is soluble in water, and be added in the mixed solution of above-mentioned step A, and stir.
C, in whipping process high-purity Ar or high pure nitrogen constantly are passed through, to protect the Mn in solution2+And Fe2+Not by Oxidation.The pH value of solution is tested, can be by between ammoniacal liquor regulation pH range 8 ~ 9.
D, stir after, mixed system is transferred in reactor, and between 150 ~ 180 DEG C hydro-thermal reaction 8 ~ 12h, after the completion of reaction, precipitated product centrifuge washing is dried;
E, then sediment and carbon source are mixed, the amount of carbon source is 1%- according to the content of carbon in final product 15% addition, after grinding is uniform, under conditions of inert gas shielding is passed through, calcines 2h, then temperature liter at 250 DEG C first Between high to 600 DEG C ~ 800 DEG C, 4 ~ 12h is calcined, the material of final product lithium ferric manganese phosphate carbon coated is obtained.
In such scheme, the additive is cetyl trimethylammonium bromide, ethylenediamine tetra-acetic acid, polyvinylpyrrolidine One or more of which in ketone.
The manganese source is one kind in manganese sulfate, manganese nitrate, manganese acetate, manganese chloride etc..
The source of iron is one kind in ferrous sulfate, iron ammonium sulfate, ferrous nitrate, frerrous chloride etc..
The lithium source is one kind in lithium hydroxide, lithium acetate, lithium sulfate, lithium nitrate etc..
Phosphorus source uses one or more therein in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate.
The carbon source uses glucose, sucrose, starch, cellulose, pyrroles, fructose, acetylene black, Super P, polystyrene Etc. one or more therein.
The solution have the advantages that:Prepared using hydro-thermal method, obtain a kind of lithium ferric manganese phosphate material of cuboid-type, grain Footpath is about that between 50-500nm, the structure of cuboid can make Li in charge and discharge process+Along b direction of principal axis ordered movements, have Beneficial to the insertion and abjection of lithium ion, so as to improve Li+The kinetics of motion, improves ionic conductivity.Pass through Two step carbon coatings, obtain lithium ferric manganese phosphate cladding carbon material, the electrical conductivity of material, enhancing are improved after carbon coated after calcining The electric conductivity of material.Obtained material first discharge specific capacity can reach more than 140mAh/g, 1C specific discharge capacity energy 130mAh/g is reached, 5C specific discharge capacities can reach more than 110mAh/g, show preferable high rate performance.
Special rectangular parallelepiped structure serves very big positive role for the lifting of material final performance.
The present invention is by adding the additives such as surfactant or complexing agent, and additive passes through ionic bond or hydrogen bond and life Into microcrystal grain nucleus link together, influence crystal grain a direction growth, it is grown along specific direction so that Form the product of specific morphology.In addition, the electrostatic effect and space steric effect of additive can prevent particle from rolling into a ball in the liquid phase It is poly-, powder is kept preferable single dispersing.It is easy and effective, convenient and swift and cost is relatively low.
The invention will be further described with reference to the accompanying drawings and examples.
Brief description of the drawings
Accompanying drawing 1 is product LiFe in the embodiment of the present invention 10.2Mn0.8PO4/ C SEM figures;
Accompanying drawing 2 is product LiFe in the embodiment of the present invention 20.2Mn0.8PO4/ C SEM figures;
Accompanying drawing 3 is product LiFe in the embodiment of the present invention 10.2Mn0.8PO4/ C XRD;
Accompanying drawing 4 is product LiFe in the embodiment of the present invention 10.2Mn0.8PO4/ C 0.1C discharge curves first;
Accompanying drawing 5 is product LiFe in the embodiment of the present invention 10.2Mn0.8PO4/ C 1C cycle life curve maps;
Accompanying drawing 6 is product LiFe in the embodiment of the present invention 10.2Mn0.8PO4/ C high rate performance curve map.
Embodiment
Embodiment 1:A kind of preparation method of cuboid-type lithium battery lithium ferric manganese phosphate positive electrode, comprises the following steps: 2.0402g lithium acetate is dissolved in 20ml water, 2.7043g manganese sulfate is dissolved in 20ml water, by 1.5686g ferrous sulfate Ammonium is added in manganese sulfate solution, and stirring is to dissolving, and the process of dissolving and stirring mixing is passed through inert gas shielding, will In 2.3006g ammonium dihydrogen phosphate 20nl water, lithium salt solution, phosphorus source solution and manganese source, source of iron mixed solution are mixed equal It is even.
0.5g CTAB is dissolved in 15ml water, and adds 5ml ethylene glycol, CTAB solution is then added to mixture In system, it is 8.5 with ammoniacal liquor regulation pH value, mixed solution is transferred in reactor, 8h is reacted at 180 DEG C, after the completion of reaction, Pelleting centrifugation is washed, dried, then intermediate product and 0.6986g glucose are mixed, after grinding is uniform, forged at high temperature Burn, calcine 2h at 250 DEG C first, be then raised to 800 DEG C, calcine 4h, obtain lithium ferric manganese phosphate bag carbon material.
Accompanying drawing 1 is the SEM figures for the product that embodiment 1 is obtained, it is evident that pattern is cuboid-type, and accompanying drawing 3 is to obtain product XRD, obtained diffraction maximum is consistent with the standard diagram of lithium ferric manganese phosphate, occurs without impurity peaks, illustrates obtained product It is purer.
With obtained product as positive electrode, using metal lithium sheet as to electrode, using 32 μm of barrier film, electrolyte is adopted With the LiPF for the 1mol/L that solvent is EC, DMC, EMC6Electrolyte, is assembled into CR2025 type button cells in glove box, uses LAND CT2001A battery test system button types battery carries out electric performance test, and voltage range is 2.5 ~ 4.5V, current density For 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 capacities reach 140mAh/g More than, under the conditions of 1C, after 80 times circulate, specific capacity can also reach more than 120mAh/g, even if multiplying power reaches 5C, specific capacity Also in more than 110mAh/g.
Embodiment 2:A kind of preparation method of cuboid-type lithium battery lithium ferric manganese phosphate positive electrode, comprises the following steps:
2.0402g lithium acetate is dissolved in 20ml water, 2.7043g manganese sulfate is dissolved in 20ml water, by 1.5686g's Iron ammonium sulfate is added in manganese sulfate solution, and stirring is to dissolving, and the process of dissolving and stirring mixing is passed through inert gas shielding, By in 2.3006g ammonium dihydrogen phosphate 20nl water, lithium salt solution, phosphorus source solution and manganese source, source of iron mixed solution are mixed Uniformly.0.5g EDTA is dissolved in 15ml water, and adds 5ml ethylene glycol, EDTA solution is then added to mixed system In, it is 8.5 with ammoniacal liquor regulation pH value, mixed solution is transferred in reactor, 10h is reacted at 170 DEG C, after the completion of reaction, Pelleting centrifugation is washed, dried, then intermediate product and 0.6168g glucose are mixed, after grinding is uniform, forged at high temperature Burn, calcine 2h at 250 DEG C first, be then raised to 700 DEG C, calcine 8h, obtain lithium ferric manganese phosphate bag carbon material.
Accompanying drawing 2 is the SEM figures for the product that embodiment 2 is obtained, it is evident that pattern is the cuboid-type of rule, its XRD With embodiment 1 obtain it is consistent, as a result see accompanying drawing 3.
Embodiment 3:A kind of preparation method of cuboid-type lithium battery lithium ferric manganese phosphate positive electrode, comprises the following steps:
2.0402g lithium acetate is dissolved in 20ml water, 2.7043g manganese sulfate is dissolved in 20ml water, by 1.5686g's Iron ammonium sulfate is added in manganese sulfate solution, and stirring is to dissolving, and the process of dissolving and stirring mixing is passed through inert gas shielding, By in 2.3006g ammonium dihydrogen phosphate 20nl water, lithium salt solution, phosphorus source solution and manganese source, source of iron mixed solution are mixed Uniformly.0.5g CTAB is dissolved in 15ml water, and adds 5ml ethylene glycol, CTAB solution is then added to mixed system In, it is 8.5 with ammoniacal liquor regulation pH value, mixed solution is transferred in reactor, 12h is reacted at 150 DEG C, after the completion of reaction, Pelleting centrifugation is washed, dried, then intermediate product and 0.7504g glucose are mixed, after grinding is uniform, forged at high temperature Burn, calcine 2h at 250 DEG C first, be then raised to 600 DEG C, calcine 12h, obtain lithium ferric manganese phosphate bag carbon material.
Following table is the technological parameter in above-described embodiment:

Claims (7)

1. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate, it is characterised in that:By persursor material Manganese source compound, Fe source compound, P source compound and Li source compound, by Mn:Fe:P:Li elemental mole ratios are 0.8:0.2: 1:3 weigh and are dissolved in water respectively, additive mixed dissolution are then added, by each under conditions of inert gas shielding is passed through Solution is well mixed, and heating response is carried out in a kettle., is finally mixed with appropriate carbon source, is ground, is calcined successively, is produced Thing lithium ferric manganese phosphate bag carbon composite;
This method comprises the following steps:
Persursor material manganese source compound, Fe source compound, P source compound and Li source compound are pressed into Mn:Fe:P:Li elements Mol ratio is 0.8:0.2:1:3 weigh, and are dissolved in water formation 1mol/L solution respectively;
Manganese source and source of iron are mixed, phosphorus source and lithium source are well mixed, 0.5g additive is dissolved in 20ml water, surface is used as In activating agent or complexing agent, the mixed solution that additive solution is added to ferromanganese source, and stir, be then added to phosphorus source Stirred in the mixed liquor of lithium source, and constantly;
Inert gas constantly is passed through in stirring mixed process, to protect the Mn in solution2+And Fe2+It is not oxidized;
The pH value of solution is tested, and by between ammoniacal liquor regulation pH range 8 ~ 9;
Described product is cuboid-type, and particle diameter is between 50-500nm;
This method is further comprising the steps of:
After stirring, mixed system is transferred in reactor, and 8 ~ 12h of hydro-thermal reaction between 150 ~ 180 DEG C, reaction After the completion of, pelleting centrifugation is washed, dried;Obtained precipitation and carbon source are mixed, after grinding is uniform, forged first at 250 DEG C 2h is burnt, is then raised between 600 DEG C ~ 800 DEG C, 4 ~ 12h is calcined, obtains product lithium ferric manganese phosphate bag carbon composite;
The additive is the one of which in cetyl trimethylammonium bromide, ethylenediamine tetra-acetic acid, polyvinylpyrrolidone Or it is a variety of.
2. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:Phosphorus source uses the one or more of which in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate.
3. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:The manganese source uses one kind in manganese sulfate, manganese nitrate, manganese acetate, manganese chloride.
4. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:The source of iron is one kind in ferrous sulfate, iron ammonium sulfate, ferrous nitrate, frerrous chloride.
5. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:The lithium source is one kind in lithium hydroxide, lithium acetate, lithium sulfate, lithium nitrate.
6. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:The carbon source uses glucose, sucrose, starch, cellulose, pyrroles, fructose, acetylene black, Super P, polystyrene One or more therein.
7. a kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate according to claim 1, it is special Levy and be:The pH value of described solution ammoniacal liquor regulated value 8 ~ 9.
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