CN104347852A - Preparation method of lithium manganese phosphate-lithium vanadium phosphate composite material - Google Patents
Preparation method of lithium manganese phosphate-lithium vanadium phosphate composite material Download PDFInfo
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- CN104347852A CN104347852A CN201410485884.4A CN201410485884A CN104347852A CN 104347852 A CN104347852 A CN 104347852A CN 201410485884 A CN201410485884 A CN 201410485884A CN 104347852 A CN104347852 A CN 104347852A
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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
- H01M4/362—Composites
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of a lithium manganese phosphate-lithium vanadium phosphate composite material. The preparation method comprises the steps of adding 0.1-0.4mol/L of ammonium metavanadate solutions to a reaction kettle containing 0.05-0.20mol/L of manganese acetate solution at the speed of 0.5-2.0L/hour; controlling the final mole ratio of manganese element to vanadium elements, namely Mn to V being, 1 to 2, and controlling reaction temperature to be 50-90 DEG C and stirring speed to be 200-1200rpm; after feeding is completed, regulating the pH of a solution to be 4-7, and standing; filtering, washing, and then drying to obtain MnV2O6.2H2O; mixing MnV2O6.2H2O, a lithium source compound, a phosphorus source compound and a composite carbon source at the proportion of mole ratio of manganese element to vanadium element to phosphorus element to lithium element to carbon element being 1 to 2 to 4 to 4 to (0.1-10), carrying out ball-milling, drying, and sintering so as to form the lithium manganese phosphate-lithium vanadium phosphate composite material. The preparation method disclosed by the invention has simple process flow; the obtained product has the advantages of good and stable quality and low cost and is especially suitable for being applied to a higher-voltage platform lithium ion battery.
Description
Technical field
The present invention relates to the preparation method of a kind of lithium manganese phosphate-phosphoric acid vanadium lithium composite material, particularly a kind of preparation method being used as the lithium manganese phosphate-phosphoric acid vanadium lithium composite material of anode material for lithium-ion batteries.
Background technology
Along with the consumption gradually of the main natural resources such as coal, oil, the arrival of energy crisis causes increasing concern.In this context, the novel high-energy chemical power source of green non-pollution has become the focus competitively developed countries in the world.
Lithium ion battery is a kind of novel chemical power source, reversibly embeds respectively and the compound of deviating from lithium ion is formed as both positive and negative polarity with two.When battery charges, lithium ion deintercalation from positive pole out, embeds in negative pole; During electric discharge, lithium ion deintercalation from negative pole out, embeds in positive pole.Lithium ion battery is owing to having high-energy-density, high voltage, pollution-free, and the advantages such as cycle life is high, memory-less effect, have been widely used in notebook computer, mobile phone and other portable electronics at present.
Existing Postive electrode material of li-ion accumulator mainly contains cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary system and phosphate system positive electrode.Wherein, cobalt acid lithium, nickel-cobalt-manganese ternary system and phosphate system positive electrode are mainstay material, but in cobalt acid lithium, cobalt toxicity is comparatively large, and cobalt resource is seriously rare, expensive.Nickel-cobalt-manganese ternary material at high temperature stability inferior can reduce owing to producing oxygen, and causes potential safety hazard.And though the LiFePO 4 material in phosphate system has good thermal stability (thermal discharge is 260J/g), the lower 3.4V of voltage platform, limits its power output, and its conductivity is very low by (~ 10
-9s).Concerning the lithium ion battery requiring more high power capacity, cheap price, higher platform is that development is necessary.
Lithium manganese phosphate is the another kind of important electrode material of olivine structural phosphate family, reported first is taught by Goodenough in 1997, lithium manganese phosphate has the discharge platform (4.1V) of cheap price and Geng Gao, similar theoretical capacity 170mAh/g, its poor conductivity (10
-10s) also improving by material preparation technology, is the advantageous material as improving workbench.
Phosphoric acid vanadium lithium is the compound of monocline, and being considered to may be polyanionic positive electrode more better than LiFePO4 performance.Phosphoric acid vanadium lithium, owing to having the advantage such as theoretical specific capacity high (197mAh/g), cryogenic property and Heat stability is good, cycle performance excellence, cost, is subject to extensive concern.
Research shows, lithium manganese phosphate-phosphoric acid vanadium lithium the composite material with olivine structural and monocline two kinds of principal goods phases combines both performances, have that discharge platform is high and stable, high rate performance is excellent, theoretical specific capacity high (between 170mAh/g and 197mAh/g), Heat stability is good, the feature such as cheap, environmental friendliness, meet the important development direction of current anode material for lithium-ion batteries.
But, less about the correlative study that lithium manganese phosphate-prepared by phosphoric acid vanadium lithium composite material at present.
Summary of the invention
Technical problem to be solved by this invention is, provides the preparation method of a kind of lithium manganese phosphate-phosphoric acid vanadium lithium composite material.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of a kind of lithium manganese phosphate-phosphoric acid vanadium lithium composite material, comprises the following steps:
(1) ammonium metavanadate solution of 0.1 ~ 0.4mol/L is added to the speed of 0.5 ~ 2.0L/h in the reactor filling 0.05 ~ 0.20mol/L manganese acetate solution, control final manganese, v element mol ratio is Mn:V=1:2, to control reaction temperature be 50 ~ 90 DEG C and mixing speed is 200 ~ 1200rpm;
(2) after having fed in raw material, add ammoniacal liquor regulate pH value of solution to 4 ~ 7, leave standstill 0.5 ~ 12h, after filtration, washing after, at blast drier in 70 ~ 120 DEG C of drying 10 ~ 13h, obtain MnV
2o
62H
2o;
(3) with MnV
2o
62H
2o, Li source compound, P source compound and compounded carbons are raw material, be the proportioning of 1:2:4:4:0.1 ~ 10 by manganese, vanadium, phosphorus, lithium, carbon mol ratio, take absolute ethyl alcohol as decentralized medium, ball milling 4 ~ 12h under 200 ~ 400rpm, again in 50 ~ 70 DEG C of drying 10 ~ 13h, obtain precursor material;
(4) under protective gas atmosphere in 400 ~ 800 DEG C of roasting 10 ~ 20h, obtain the lithium manganese phosphate-phosphoric acid vanadium lithium composite material of excellent performance.
Further, in step (3), described Li source compound is lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or lithium nitrate.
Further, in step (3), described P source compound is ammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, lithium dihydrogen phosphate, tertiary sodium phosphate, triethyl phosphate, tributyl phosphate or phosphate.
Further, in step (3), described compounded carbons is in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenolic resins, acrylic resin, epoxy resin, oxalic acid or citric acid two or three.
Further, in step (4), described protective gas is argon gas, nitrogen, hydrogen, hydrogen and argon gas gaseous mixture (density of hydrogen 1% ~ 80%), carbon dioxide or carbon monoxide.
Utilize the product electrochemical performance that gained composite material of the present invention is obtained, its 0.1C first discharge specific capacity can be 121.8mAh/g, 1C first discharge specific capacity is 0.1C first discharge specific capacity 99.4%, 2C first discharge specific capacity is 93.7% of 0.1C first discharge specific capacity, 5C first discharge specific capacity is 90.0% of 0.1C first discharge specific capacity, high rate performance is excellent, circulate under 0.1C to still have after 30 times 99.3% capacity.
Raw material sources of the present invention are wide, and technological process is simple, good product quality and stable, and cost is low, is particularly suitable for the application of high voltage platform lithium ion battery.
Accompanying drawing explanation
The XRD collection of illustrative plates of Fig. 1 lithium manganese phosphate obtained by embodiment 1-phosphoric acid vanadium lithium composite material;
The SEM collection of illustrative plates of Fig. 2 lithium manganese phosphate obtained by embodiment 1-phosphoric acid vanadium lithium composite material;
The charging and discharging curve figure of Fig. 3 lithium manganese phosphate obtained by embodiment 1-phosphoric acid vanadium lithium composite material under different multiplying;
The cyclic curve figure of Fig. 4 lithium manganese phosphate obtained by embodiment 1-phosphoric acid vanadium lithium composite material under 0.1C multiplying power.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
The present embodiment comprises the following steps:
(1) take four water manganese acetate 245g, be dissolved in the deionized water of 8L, take ammonium metavanadate 234g, be dissolved in the deionized water of 10L; First added in reactor by manganese acetate solution, then be added drop-wise in reactor by ammonium metavanadate solution with the speed of 1.0L/h, control mixing speed is 800rpm, and reaction temperature is 60 DEG C;
(2) after having fed in raw material, with ammoniacal liquor regulate pH value of solution be 6, leave standstill 6h, after filtration, washing after, at blast drier in 80 DEG C of dry 12h, obtain 288g MnV
2o
62H
2o;
(3) MnV is taken
2o
62H
2o 288g, lithium dihydrogen phosphate 416g, glucose 50g, oxalic acid 150g, be carry out the activation of mechanical ball mill after medium mixing with absolute ethyl alcohol, soak time is 8 h, ball milling speed is 300 rpm, dry 12h in 60 DEG C of convection oven again, obtains lithium manganese phosphate-phosphoric acid vanadium lithium composite material precursor;
(4) 650 DEG C are heated in a nitrogen atmosphere, and constant temperature calcining 15h, cool to room temperature with the furnace subsequently, obtain the lithium manganese phosphate-phosphoric acid vanadium lithium composite positive pole of excellent performance.
The XRD collection of illustrative plates of the present embodiment gained lithium manganese phosphate-phosphoric acid vanadium lithium composite material, as shown in Figure 1; The SEM collection of illustrative plates of gained lithium manganese phosphate-phosphoric acid vanadium lithium composite material, as shown in Figure 2.
The assembling of battery: the lithium manganese phosphate-phosphoric acid vanadium lithium composite positive pole taking 0.40g gained, add 0.05 g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025, wherein, charging and discharging curve figure under different multiplying, as shown in Figure 3, as shown in Figure 3,0.1C first discharge specific capacity is 121.8mAh/g, 1C first discharge specific capacity is 121.0mAh/g, 2C first discharge specific capacity be 114.1mAh/g, 5C first discharge specific capacity is 109.1mAh/g; Cyclic curve figure under 0.1C multiplying power, as shown in Figure 4, circulates after 30 times and still has 120.9mAh/g under 0.1C.
embodiment 2
The present embodiment comprises the following steps:
(1) take four water manganese acetate 122.55g, be dissolved in the deionized water of 5L, take ammonium metavanadate 117.00g, be dissolved in the deionized water of 10L; First added in reactor by manganese acetate solution, then be added drop-wise in reactor by ammonium metavanadate solution with the speed of 0.5L/h, control mixing speed is 1200rpm, and reaction temperature is 50 DEG C;
(2) after having fed in raw material, with ammoniacal liquor regulate pH value of solution be 4, leave standstill 0.5h, after filtration, washing after, at blast drier in 85 DEG C of dry 12h, obtain 142.00g MnV
2o
62H
2o;
(3) MnV is taken
2o
62H
2o 142.00g, lithium hydroxide 48g, ammonium hydrogen phosphate 264g, shitosan 80g, malic acid 100g, be carry out the activation of mechanical ball mill after medium mixing with absolute ethyl alcohol, soak time is 4h, ball milling speed is 250rpm, dry 11h in 55 DEG C of baking ovens again, obtains lithium manganese phosphate-phosphoric acid vanadium lithium composite material precursor;
(4) be heated to 600 DEG C under an argon atmosphere, and constant temperature calcining 10h, subsequently by air cooling to room temperature, obtain the lithium manganese phosphate-phosphoric acid vanadium lithium composite material of excellent performance.
The assembling of battery: the lithium manganese phosphate-phosphoric acid vanadium lithium composite material taking 0.40g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, after mixing, be coated on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025,0.1C first discharge specific capacity is 118.8mAh/g, 1C first discharge specific capacity is 117.0mAh/g, circulate after 30 times and still have 115.8mAh/g, 2C first discharge specific capacity is 110.1mAh/g, 5C first discharge specific capacity is 106.1mAh/g.
embodiment 3
The present embodiment comprises the following steps:
(1) take four water manganese acetate 490g, be dissolved in the deionized water of 8L, take ammonium metavanadate 468g, be dissolved in the deionized water of 10L; First added in reactor by manganese acetate solution, then be added drop-wise in reactor by ammonium metavanadate solution with the speed of 2.0L/h, control mixing speed is 200rpm, and reaction temperature is 90 DEG C;
(2) after having fed in raw material, with ammoniacal liquor regulate pH value of solution be 7, leave standstill 12h, after filtration, washing after, at blast drier in 80 DEG C of dry 12h, obtain 576 g MnV
2o
62H
2o;
(3) MnV is taken
2o
62H
2o 576g, lithium carbonate 296g, ammonium dihydrogen phosphate 928g, acetic acid 150g, phenolic resins 200g, be carry out the activation of mechanical ball mill after medium mixing with absolute ethyl alcohol, soak time is 12h, ball milling speed is 400rpm, dry 13h in 60 DEG C of baking ovens again, obtains lithium manganese phosphate-phosphoric acid vanadium lithium composite material precursor;
(4) be heated to 800 DEG C in a nitrogen atmosphere, and constant temperature calcining 20h, subsequently by air cooling to room temperature, obtain the lithium manganese phosphate-phosphoric acid vanadium lithium composite material of excellent performance.
The assembling of battery: the lithium manganese phosphate-phosphoric acid vanadium lithium composite material taking 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, after mixing, be coated on aluminium foil and make positive plate, be negative pole with metal lithium sheet in vacuum glove box, with Celgard 2300 for barrier film, 1mol/L LiPF
6/ EC: DMC(volume ratio 1: 1) be electrolyte, can be assembled into the button cell of CR2025,0.1C first discharge specific capacity is 119.8mAh/g, circulate after 30 times and still have 117.8mAh/g, 1C first discharge specific capacity is 119.0mAh/g, 2C first discharge specific capacity is 109.1mAh/g, 5C first discharge specific capacity is 105.1mAh/g.
Claims (5)
1. a preparation method for lithium manganese phosphate-phosphoric acid vanadium lithium composite material, is characterized in that, comprise the following steps:
(1) ammonium metavanadate solution of 0.1 ~ 0.4mol/L is added to the speed of 0.5 ~ 2.0L/h in the reactor filling 0.05 ~ 0.20mol/L manganese acetate solution, control final manganese, v element mol ratio is Mn:V=1:2, to control reaction temperature be 50 ~ 90 DEG C and mixing speed is 200 ~ 1200rpm;
(2) after having fed in raw material, add ammoniacal liquor regulate pH value of solution to 4 ~ 7, leave standstill 0.5 ~ 12h, after filtration, washing after, at blast drier in 70 ~ 120 DEG C of drying 10 ~ 13h, obtain MnV
2o
62H
2o;
(3) with MnV
2o
62H
2o, Li source compound, P source compound and compounded carbons are raw material, be the proportioning of 1:2:4:4:0.1 ~ 10 by manganese, vanadium, phosphorus, lithium, carbon mol ratio, take absolute ethyl alcohol as decentralized medium, ball milling 4 ~ 12h under 200 ~ 400rpm, again in 50 ~ 70 DEG C of drying 10 ~ 13h, obtain precursor material;
(4) under protective gas atmosphere in 400 ~ 800 DEG C of roasting 10 ~ 20h, obtain the lithium manganese phosphate-phosphoric acid vanadium lithium composite material of excellent performance.
2. the preparation method of lithium manganese phosphate according to claim 1-phosphoric acid vanadium lithium composite material, it is characterized in that: in step (3), described Li source compound is lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or lithium nitrate.
3. the preparation method of lithium manganese phosphate according to claim 1 and 2-phosphoric acid vanadium lithium composite material, it is characterized in that: in step (3), described P source compound is ammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, lithium dihydrogen phosphate, tertiary sodium phosphate, triethyl phosphate, tributyl phosphate or phosphate.
4. the preparation method of lithium manganese phosphate according to claim 1 and 2-phosphoric acid vanadium lithium composite material, it is characterized in that: in step (3), described compounded carbons is in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenolic resins, acrylic resin, epoxy resin, oxalic acid or citric acid two or three.
5. the preparation method of lithium manganese phosphate according to claim 1 and 2-phosphoric acid vanadium lithium composite material, is characterized in that: in step (4), and described protective gas is argon gas, nitrogen, hydrogen, hydrogen and argon gas gaseous mixture, carbon dioxide or carbon monoxide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104916840A (en) * | 2015-05-08 | 2015-09-16 | 武汉理工大学 | Three-dimensional porous grading carbon modified LMP-LVP/C electrode material, and preparation method and application thereof |
| CN105280917A (en) * | 2015-09-22 | 2016-01-27 | 中南大学 | Preparation method of nano-MnV2O6 anode material |
| CN112028123A (en) * | 2020-09-15 | 2020-12-04 | 广东工业大学 | Preparation method of manganese vanadate material and energy storage application thereof |
| CN113060716A (en) * | 2021-03-26 | 2021-07-02 | 天津斯科兰德科技有限公司 | Preparation method of manganese vanadium lithium phosphate cathode material |
| CN114242988A (en) * | 2021-12-28 | 2022-03-25 | 湖北亿纬动力有限公司 | Positive electrode material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104916840A (en) * | 2015-05-08 | 2015-09-16 | 武汉理工大学 | Three-dimensional porous grading carbon modified LMP-LVP/C electrode material, and preparation method and application thereof |
| CN105280917A (en) * | 2015-09-22 | 2016-01-27 | 中南大学 | Preparation method of nano-MnV2O6 anode material |
| CN112028123A (en) * | 2020-09-15 | 2020-12-04 | 广东工业大学 | Preparation method of manganese vanadate material and energy storage application thereof |
| CN112028123B (en) * | 2020-09-15 | 2023-03-28 | 广东工业大学 | Preparation method of manganese vanadate material and energy storage application thereof |
| CN113060716A (en) * | 2021-03-26 | 2021-07-02 | 天津斯科兰德科技有限公司 | Preparation method of manganese vanadium lithium phosphate cathode material |
| CN113060716B (en) * | 2021-03-26 | 2022-12-13 | 天津斯科兰德科技有限公司 | Preparation method of manganese vanadium lithium phosphate cathode material |
| CN114242988A (en) * | 2021-12-28 | 2022-03-25 | 湖北亿纬动力有限公司 | Positive electrode material and preparation method and application thereof |
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Application publication date: 20150211 |