CN104241645A - Synthesis method of lithium-manganese-phosphate anode material - Google Patents
Synthesis method of lithium-manganese-phosphate anode material Download PDFInfo
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- CN104241645A CN104241645A CN201410176020.4A CN201410176020A CN104241645A CN 104241645 A CN104241645 A CN 104241645A CN 201410176020 A CN201410176020 A CN 201410176020A CN 104241645 A CN104241645 A CN 104241645A
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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
- H01M4/364—Composites as mixtures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a synthesis method of a lithium-manganese-phosphate anode material. The synthesis method is characterized by comprising the steps of liquefying low-melt-point reaction materials, then mixing the liquefied materials by utilizing the difference of the reaction materials and generated materials in melt points, uniformly mixing lithium, manganese and phosphorus at a molecular scale, separating out a high-melt-point product to obtain an ultrafine crystal lithium-manganese-phosphorus precursor, washing the ultrafine crystal lithium-manganese-phosphorus precursor by utilizing water to simply remove side products, adding carbon sources such as sugarcane and glucose, uniformly mixing the ultrafine crystal lithium-manganese-phosphorus precursor with the carbon source to form a solid phase, and sintering the mixture to obtain a lithium-manganese-phosphate product with excellent performance. The synthesized lithium-manganese-phosphate material has the characteristics of small grain size, high capacity, good multiplying power and the like. Compared with a hydrothermal method, the synthesis method is more energy-saving and environment-friendly, simple and easy in the entire process and applicable to mass production.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries production technical field, particularly a kind of synthetic method of manganese-lithium phosphate anode material.
Background technology
Lithium manganese phosphate is as the positive electrode of power lithium-ion battery, there is the advantages such as voltage is high, fail safe good, the life-span is long, cost is low, aboundresources, energy density promotes more than 20% than LiFePO4, be a kind of positive electrode having application prospect, be considered to one of optimal selection of power lithium-ion battery of future generation.
The preparation method that patent discloses a kind of manganese-lithium phosphate anode material of publication number CN 103413943A; be that 1 ~ 1.2:1 takes phosphorus source and manganese source material in molar ratio; get 5-15% carbon-source cpd and the 1-10% surfactant of this phosphorus source and manganese source material quality summation again; be made into the suspension that solid content is 10 ~ 50%; filter after hydro-thermal reaction, wash dry square manganese phosphate precursor; fully mix with lithium source again, naturally cool after high temperature sintering under nitrogen atmosphere protection.The solid-state mixing of what the method was taked is raw material, the defect of existence is that the mixture homogeneity of raw material is inadequate, and the lithium manganese phosphate crystallite dimension of formation is large and uneven, poor electrical performance.And hydro-thermal rule equipment requirement is high, high pressure-temperature reacts, and safety causes anxiety, and waste water is many, the excessive configuration of lithium, and waste is large, and large-scale production difficulty is large.And can not adulterate, can not prepare the lithium manganese phosphate material of non-stoichiometric, limitation is large. simultaneously
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of manganese-lithium phosphate anode material, adopt liquid phase mixed method to realize the molecule rank Homogeneous phase mixing of lithium, manganese, phosphorus three kinds of elements, the lithium manganese phosphate material of synthesis has the features such as crystallite dimension is little, capacity is high, multiplying power is good.Compared to the energy-conserving and environment-protective more of hydro-thermal rule, whole process is simple and easy to do, is applicable to large-scale production.
The technical solution adopted for the present invention to solve the technical problems is:
A synthetic method for manganese-lithium phosphate anode material, comprises the following steps:
(1) ratio of Lithium acetate dihydrate and four water acetic acid manganese 1:1 is in molar ratio mixed, be heated to 80 DEG C-100 DEG C liquefaction under then under stirring condition, obtain liquid A; Phosphorus source is heated to 80 DEG C-100 DEG C liquefaction, obtains liquid B;
(2) by lithium: manganese: the mol ratio 1:1:1 of phosphorus, under stirring condition, liquid A is slowly added in liquid B and obtains suspension-turbid liquid C, then continue to stir 10-120 minute, a standing 30-120 point clock aging obtains presoma, keeps system temperature in whole process between 80 DEG C-100 DEG C;
(3) presoma is added water, clean 3-5 time;
(4) presoma after cleaning is dried at 80 DEG C-180 DEG C moisture content less than 5% and obtains dry presoma;
(5) by the presoma of drying and carbon source mixing and ball milling 2-8h, finally 500 DEG C-800 DEG C sintering 0.5-12 hour in inert atmosphere, obtain manganese-lithium phosphate anode material.
Selection Lithium acetate dihydrate, four water acetic acid manganese are the reason of raw material is that (80 DEG C-100 DEG C) easily liquefy at a lower temperature because the fusing point of these two raw materials is low.
Select ten phosphate dihydrate sodium (Na
3pO
412H
2or sodium dihydrogen phosphate dihydrate (NaH O)
2pO
42H
2o) be phosphorus source, phosphorus source must contain the crystallization water, and such fusing point is low, and more than 80 DEG C just can be melted into liquid state.
After synthesis presoma, utilize presoma water insoluble, and the feature that accessory substance is water-soluble, simply can remove accessory substance.
Principle of the present invention utilizes reactive material (lithium source, manganese source, phosphorus source) and the difference generating material (lithium manganese phosphate presoma) fusing point, by low melting point reaction mass post liquefaction is mixed, realize the molecule rank Homogeneous phase mixing of lithium, manganese, phosphorus three kinds of elements, high-melting-point product is separated out and is obtained Ultra-fine Grained lithium manganese phosphorus presoma simultaneously, again can simply except removing accessory substance with water cleaning, add the carbon source such as sucrose, glucose, mix the lithium manganese phosphate product that rear solid-phase sintering can obtain function admirable.
Raw material of the present invention is mixed by liquid liquid, lithium without the need to excessive configuration, basic free of losses.And the present invention can adulterate when raw material mixes simultaneously, easy and simple to handle.
As preferably, phosphorus source described in step (1) is ten phosphate dihydrate sodium or sodium dihydrogen phosphate dihydrates.
As preferably, in step (3) consumption of water be the 1-2 of presoma weight doubly.
As preferably, in step (3), clean is specially under stirring condition and filters after sonic oscillation 5-30min.Sonic oscillation can make cleaning more thorough, and it is more thorough that accessory substance is removed.
As preferably, mixing speed is 20-120rpm.
As preferably, in step (5), carbon source consumption is the 1%-15% of dry presoma weight.
As preferably, carbon source described in step (5) selects the one in glucose, sucrose, carbon black, carbon nano-tube, Graphene.
The invention has the beneficial effects as follows:
1, by low melting point reaction mass post liquefaction is mixed, realize the molecule rank Homogeneous phase mixing of lithium, manganese, phosphorus three kinds of elements, high-melting-point product is separated out and is obtained Ultra-fine Grained lithium manganese phosphorus presoma simultaneously, again can simply except removing accessory substance with water cleaning, add carbon source, mix the lithium manganese phosphate product that rear solid-phase sintering can obtain function admirable.
2, the lithium manganese phosphate material of synthesis has the features such as crystallite dimension is little, capacity is high, multiplying power is good.Compared to the energy-conserving and environment-protective more of hydro-thermal rule, whole process is simple and easy to do, is applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the TEM figure of lithium manganese phosphate material of the present invention.
Embodiment
Below by specific embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1:
A synthetic method for manganese-lithium phosphate anode material, comprises the following steps:
(1) ratio of Lithium acetate dihydrate and four water acetic acid manganese 1:1 is in molar ratio mixed, be heated to 80 DEG C of liquefaction under then under stirring condition, obtain light red transparency liquid A; Ten phosphate dihydrate sodium are heated to 80 DEG C of liquefaction, obtain liquid B.
(2) by lithium: manganese: the mol ratio 1:1:1 of phosphorus, under stirring condition, liquid A is slowly added in liquid B the suspension-turbid liquid C obtaining taupe, then continue stirring 120 minutes, leave standstill 120 points of clock agings and obtain presoma, in whole process, keep system temperature between 80 DEG C-90 DEG C.
(3) presoma is added the water of equivalent weight, clean 5 times, clean is specially under the stirring condition of 120rpm rotating speed and filters after sonic oscillation 5min.
(4) presoma after cleaning is dried at 80 DEG C moisture content less than 5% and obtains dry presoma.
(5) by the Graphene mixing and ball milling 8h of the presoma of drying with dry presoma weight 1%, finally 500 DEG C of sintering 12 hours in nitrogen atmosphere, obtain manganese-lithium phosphate anode material.
Embodiment 2:
A synthetic method for manganese-lithium phosphate anode material, comprises the following steps:
(1) ratio of Lithium acetate dihydrate and four water acetic acid manganese 1:1 is in molar ratio mixed, be heated to 100 DEG C of liquefaction under then under stirring condition, obtain light red transparency liquid A; Sodium dihydrogen phosphate dihydrate is heated to 100 DEG C of liquefaction, obtains liquid B.
(2) by lithium: manganese: the mol ratio 1:1:1 of phosphorus, under stirring condition, liquid A is slowly added in liquid B the suspension-turbid liquid C obtaining taupe, then continue stirring 10 minutes, leave standstill 30 points of clock agings and obtain presoma, in whole process, keep system temperature between 90 DEG C-100 DEG C.
(3) presoma is added the water of 2 times of weight, clean 3 times, clean is specially under the stirring condition of 20rpm rotating speed and filters after sonic oscillation 30min.
(4) presoma after cleaning is dried at 180 DEG C moisture content less than 5% and obtains dry presoma.
(5) by the glucose mixing and ball milling 2h of the presoma of drying with dry presoma weight 15%, finally 800 DEG C of sintering 0.5 hour in nitrogen atmosphere, obtain manganese-lithium phosphate anode material.
Embodiment 3:
A synthetic method for manganese-lithium phosphate anode material, comprises the following steps:
(1) ratio of Lithium acetate dihydrate and four water acetic acid manganese 1:1 is in molar ratio mixed, be heated to 90 DEG C of liquefaction under then under stirring condition, obtain light red transparency liquid A; Ten phosphate dihydrate sodium or sodium dihydrogen phosphate dihydrate are heated to 90 DEG C of liquefaction, obtain liquid B.
(2) by lithium: manganese: the mol ratio 1:1:1 of phosphorus, under stirring condition, liquid A is slowly added in liquid B the suspension-turbid liquid C obtaining taupe, then continue stirring 60 minutes, leave standstill 60 points of clock agings and obtain presoma, in whole process, keep system temperature between 85 DEG C-95 DEG C.
(3) presoma is added the water of 2 times of weight, clean 4 times, clean is specially under the stirring condition of 80rpm rotating speed and filters after sonic oscillation 20min.
(4) presoma after cleaning is dried at 120 DEG C moisture content less than 5% and obtains dry presoma.
(5) by the sucrose mixing and ball milling 4h of the presoma of drying with dry presoma weight 8%, finally 650 DEG C of sintering 5 hours in nitrogen atmosphere, obtain manganese-lithium phosphate anode material.
Performance test:
The features such as lithium manganese phosphate material has crystallite dimension little (see accompanying drawing 1), capacity is high, multiplying power is good of method synthesis of the present invention.Compared to the energy-conserving and environment-protective more of hydro-thermal rule, whole process is simple and easy to do, is applicable to large-scale production.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (7)
1. a synthetic method for manganese-lithium phosphate anode material, is characterized in that, comprises the following steps:
(1) ratio of Lithium acetate dihydrate and four water acetic acid manganese 1:1 is in molar ratio mixed, be heated to 80 DEG C-100 DEG C liquefaction under then under stirring condition, obtain liquid A; Phosphorus source is heated to 80 DEG C-100 DEG C liquefaction, obtains liquid B;
(2) by lithium: manganese: the mol ratio 1:1:1 of phosphorus, under stirring condition, liquid A is slowly added in liquid B and obtains suspension-turbid liquid C, then continue to stir 10-120 minute, a standing 30-120 point clock aging obtains presoma, keeps system temperature in whole process between 80 DEG C-100 DEG C;
(3) presoma is added water, clean 3-5 time;
(4) presoma after cleaning is dried at 80 DEG C-180 DEG C moisture content less than 5% and obtains dry presoma;
(5) by the presoma of drying and carbon source mixing and ball milling 2-8h, finally 500 DEG C-800 DEG C sintering 0.5-12 hour in inert atmosphere, obtain manganese-lithium phosphate anode material.
2. synthetic method according to claim 1, is characterized in that: phosphorus source described in step (1) is ten phosphate dihydrate sodium or sodium dihydrogen phosphate dihydrates.
3. synthetic method according to claim 1 and 2, is characterized in that: in step (3), the consumption of water is 1-2 times of presoma weight.
4. synthetic method according to claim 1 and 2, is characterized in that: clean is specially under stirring condition and filters after sonic oscillation 5-30min in step (3).
5. synthetic method according to claim 4, is characterized in that: mixing speed is 20-120rpm.
6. synthetic method according to claim 1 and 2, is characterized in that: in step (5), carbon source consumption is the 1%-15% of dry presoma weight.
7. synthetic method according to claim 1 and 2, is characterized in that: carbon source described in step (5) selects the one in glucose, sucrose, carbon black, carbon nano-tube, Graphene.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105161718A (en) * | 2015-08-03 | 2015-12-16 | 山东威能环保电源科技股份有限公司 | Preparation method for lithium battery positive material LiMnPO4 |
| CN110492060A (en) * | 2018-05-14 | 2019-11-22 | 中南大学 | A kind of differentiating stage lithium manganese phosphate/carbon composite anode material preparation method of receiving |
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| CN102593451A (en) * | 2012-03-12 | 2012-07-18 | 中国科学院过程工程研究所 | Lithium manganese phosphate nanofiber as anode material of lithium ion battery and preparation method of lithium manganese phosphate nanofiber |
| CN102664259A (en) * | 2012-05-02 | 2012-09-12 | 中国科学院宁波材料技术与工程研究所 | Method for preparing cathode material of lithium ion battery |
| CN102856540A (en) * | 2012-10-06 | 2013-01-02 | 桂林理工大学 | Method for rapid synthesis of multi-element layered positive material of lithium-ion battery |
| CN102956891A (en) * | 2011-08-26 | 2013-03-06 | 比亚迪股份有限公司 | Preparation method of lithium ion battery cathode active material Fe3O4/C, cathode and lithium ion battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102956891A (en) * | 2011-08-26 | 2013-03-06 | 比亚迪股份有限公司 | Preparation method of lithium ion battery cathode active material Fe3O4/C, cathode and lithium ion battery |
| CN102593451A (en) * | 2012-03-12 | 2012-07-18 | 中国科学院过程工程研究所 | Lithium manganese phosphate nanofiber as anode material of lithium ion battery and preparation method of lithium manganese phosphate nanofiber |
| CN102664259A (en) * | 2012-05-02 | 2012-09-12 | 中国科学院宁波材料技术与工程研究所 | Method for preparing cathode material of lithium ion battery |
| CN102856540A (en) * | 2012-10-06 | 2013-01-02 | 桂林理工大学 | Method for rapid synthesis of multi-element layered positive material of lithium-ion battery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105161718A (en) * | 2015-08-03 | 2015-12-16 | 山东威能环保电源科技股份有限公司 | Preparation method for lithium battery positive material LiMnPO4 |
| CN110492060A (en) * | 2018-05-14 | 2019-11-22 | 中南大学 | A kind of differentiating stage lithium manganese phosphate/carbon composite anode material preparation method of receiving |
| CN110492060B (en) * | 2018-05-14 | 2021-04-13 | 中南大学 | Preparation method of nano-micro grade lithium manganese phosphate/carbon composite anode material |
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