CN102646829B - Preparation method of lithium manganese silicate positive pole material - Google Patents

Preparation method of lithium manganese silicate positive pole material Download PDF

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CN102646829B
CN102646829B CN201210146626.4A CN201210146626A CN102646829B CN 102646829 B CN102646829 B CN 102646829B CN 201210146626 A CN201210146626 A CN 201210146626A CN 102646829 B CN102646829 B CN 102646829B
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lithium
manganese
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CN102646829A (en
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孙化雨
史松君
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Suzhou GCL Energy Technology Development Co Ltd
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New Materials (yancheng) Co Ltd Gcl Power
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    • 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
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    • 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 lithium ion battery positive pole material, particularly a preparation method of a lithium manganese silicate (Li2MnSiO4) positive pole material for lithium ion batteries. The preparation method comprises the following steps: adding manganese salt, lithium salt and nano silicon dioxide or ethyl orthosilicate as a reactive silicon source into an organic solvent or a mixed solution of an organic solvent and water; adding organic acid or organic amine into the solution as a pH regulator; and carrying out solvothermal reaction on the solution, washing the product, filtering, and drying to obtain the lithium manganese silicate material. The method provided by the invention can be carried out under common hydrothermal reaction kettle conditions without pressurization, thereby enhancing the safety coefficient on the premise of greatly lowering the production cost, and being convenient for industrialized large-scale production.

Description

A kind of preparation method of manganese silicate of lithium positive electrode
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries, especially relate to a kind of manganese silicate of lithium (Li for lithium ion battery 2mnSiO 4) preparation method of positive electrode.
Background technology
Li 2mnSiO 4as Olivine-type Cathode Material in Li-ion Batteries, have that theoretical specific capacity is high, good, the cheap and advantages of environment protection of Stability Analysis of Structures, cycle performance, be considered to have future the anode material for lithium-ion batteries of competitiveness, and be expected to be widely used in lithium-ion-power cell.Its traditional preparation method mainly contains high temperature solid-state method, sol-gel process and hydro thermal method etc., but the problem that these methods exist that synthesis temperature is high, the cycle long or material purity is not high and degree of crystallinity is bad.Employing microwave-the solvent-thermal methods such as T.Muraliganth in 2010 synthesize Li under 300 DEG C, 30bar pressure 2mnSiO 4material (Microwave-Solvothermal Synthesis of Nanostructured Li 2mSiO 4/ C (M=Mn and Fe) Cathodes for Lithium-Ion Batteries[J] .Chem.Mater., 2010,22 (20), 5754 – 5761), but degree of crystallinity is poor, need carry out double sintering; Recently, under the employing harsh conditions such as Devaraju M.Kempaiah, solvent-thermal method (300 DEG C/pressure of reaction temperature 38MPa) synthesizes the Li of high-purity, better crystallinity degree 2mnSiO 4material (Controlled synthesis of nanocrystalline Li2MnSiO4 particles for high capacity cathode application in lithium-ion batteries[J] Chem.Commun., 2012,48,2698 – 2700), but there is severe reaction conditions, be difficult to the problems such as control and poor reproducibility in the method.
Summary of the invention
The present invention is directed to synthetic method of the prior art and be difficult to prepare that purity is high, the technical deficiency of the manganese silicate of lithium material of better crystallinity degree, provide a kind of under the temperate condition of 150 ~ 220 DEG C, prepare the method for manganese silicate of lithium positive electrode by solvent-thermal method.
The invention provides a kind of manganese silicate of lithium (Li for lithium ion battery 2mnSiO 4) preparation method of positive electrode, concrete steps are as follows:
1) in the mixed solution of organic solvent or organic solvent and water, add manganese salt, lithium salts and nanometer grade silica or tetraethoxysilane as the silicon source of reacting;
2) in step 1) gained solution, add organic acid or organic amine as pH value conditioning agent;
3) by step 2) gained solution carries out solvent thermal reaction, and products therefrom washs, filters, is drying to obtain manganese silicate of lithium material.
Preferably, in described step 1), the charging sequence of each raw material is, first adds manganese salt, then adds lithium salts, then adds silicon dioxide or tetraethoxysilane, all tackles solution and fully stir and mix after each raw material adds.
Preferably, the organic solvent in described step 1) is ethanol or ethylene glycol, and the mixed solution of organic solvent and water is the mixed solution of second alcohol and water or the mixed solution of ethylene glycol and water.
Preferably, described organic solvent with the mixed volume ratio of water is: 8-10:1.
Preferably, in described step 1), the proportioning in manganese salt, lithium salts and silicon source is pressed the mol ratio calculating of Mn element, Li element and Si element, and the mol ratio of Mn element, Li element and Si element is: 0.7-1.3:1.4-2.6:0.7-1.3.
Preferably, in described step 1), the mol ratio of Mn element, Li element and Si element is: 0.9-1.1:0.9-1.1:0.9-1.1.
Preferably, those skilled in the art can judge the use amount of the mixed solution of described organic solvent, organic solvent and water voluntarily according to known technology.
Preferably, the volume of described organic solvent (ml) is 10:8-14 with the ratio of described silicon source, manganese salt, lithium salts weight sum (g).
Preferably, the volume of the mixed solution of organic solvent and water (ml) is 10:8-14 with the ratio of described silicon source, manganese salt, lithium salts weight sum (g).
Preferably, in described step 1), manganese salt is one or more the mixture in manganese chloride, manganese acetate, manganese carbonate or manganese sulfate.
Preferably, in described step 1), lithium salts is lithium hydroxide.
Preferably, described step 2) in organic acid be one or more the mixture in formic acid, acetic acid, citric acid or oxalic acid.
Preferably, described step 2) in organic amine be ethylenediamine.
Preferably, the reaction temperature of the solvent thermal reaction in described step 3) is 150 ~ 220 DEG C, and the reaction time is 10 ~ 48 hours.
Preferably, in described step 3), baking temperature is 90 ~ 150 DEG C.
Preferably, described step 2) the pH value=9-12 of solution of gained.
The temperature of described drying steps is high, the time is longly conducive to fully remove the adsorption solvent in material.
Second aspect present invention provides a kind of lithium ion battery manganese silicate of lithium positive electrode, is made by above-described preparation method.
The present invention adopts solvent heat, and by controlling initial reaction product mixing, pH value, reaction temperature and the reaction time of system are prepared manganese silicate of lithium material afterwards.Can be by adopting different silicon sources and different pH value conditioning agents to control target product pattern in reaction system.The high meeting of temperature Reaction time shorten in solvent thermal reaction of the present invention, reaction time deficiency can cause partial intermediate as Mn (OH) in addition 2deng and other impurity residual; In solvent thermal reaction process, being aided with magnetic agitation powder particle can be more carefully more even.
The present invention is directed to existing high temperature solid-state method, sol-gal process method, the synthetic manganese silicate of lithium material of hydro thermal method and have the problem that purity is not high, degree of crystallinity is bad or reaction condition is too harsh, provide a kind of under 150 ~ 220 DEG C of temperate conditions solvent-thermal method prepare manganese silicate of lithium positive electrode method.The method cost of material is cheap, and synthesis route is simple, and reaction condition is easy to control, and target product purity is high, and degree of crystallinity is high, and granule-morphology, fineness and particle diameter distribute to regulate and control.Especially method provided by the present invention only need can be carried out under common hydrothermal reaction kettle condition, without pressurization, has more improved coefficient of safety under the prerequisite that has significantly reduced production cost, is convenient to large-scale industrialization and produces.
Brief description of the drawings
Fig. 1 is Li prepared by the present invention 2mnSiO 4the X ray diffracting spectrum of material, test condition: the Dutch PHILIP Panalytical X-pert of company powder diffractometer (CuK alpha ray ), operating voltage 40kV, operating current is 50mA; Test parameter for be respectively angle range (°): 5 °-80 °; Step size (°): 0.0167 °; Time per step(s): 5s.
Fig. 2 is that the X ray diffracting spectrum of the each stage product of solvent thermal reaction at 220 DEG C: a is solvent thermal reaction 10h gained intermediate state mixture (Li 2mnSiO 4coexist with impurity) X ray diffracting spectrum; B is solvent thermal reaction 20h product (Li 2mnSiO 4coexist with impurity) X ray diffracting spectrum; C is solvent thermal reaction 48h product (Li 2mnSiO 4pure phase) X ray diffracting spectrum c.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
Get 9ml ethanol and 1ml water is mixed with mixed solution, add 5.200g teos solution, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 10 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
The Li of gained 2mnSiO 4the X ray diffracting spectrum of material as shown in Figure 1, test condition: the Dutch PHILIP Panalytical X-pert of company powder diffractometer (CuK alpha ray ), operating voltage 40kV, operating current is 50mA; Test parameter for be respectively angle range (°): 5 °-80 °; Step size (°): 0.0167 °; Time per step(s): 5s.
In course of reaction, as shown in Figure 2, wherein a is solvent thermal reaction 10h gained intermediate state mixture (Li to the X ray diffracting spectrum of each time period product 2mnSiO 4coexist with impurity) X ray diffracting spectrum; B is solvent thermal reaction 20h product (Li 2mnSiO 4coexist with impurity) X ray diffracting spectrum; C is solvent thermal reaction 48h product (Li 2mnSiO 4pure phase) X ray diffracting spectrum c.
Embodiment 2
Get 9ml ethanol and 1ml water is mixed with mixed solution, add 1.500g nanometer grade silica, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 12 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 3
Get 9ml ethanol and 1ml water is mixed with mixed solution, add 5.200g teos solution, stir; Add the C of 6.700g 4h 6o 4mn, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 9 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 4
Get 9ml ethanol and 1ml water is mixed with mixed solution, add 5.200g teos solution, stir; Add the MnCO of 2.875g 3, stir; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 11 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 5
Get 9ml ethanol and 1ml water is mixed with mixed solution, add 5.200g teos solution, stir; Add the MnSO of 4.225g 4, stir; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 12 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 6
Get 10ml ethanolic solution, add 5.200g teos solution, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 9 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 7
Get 10ml ethanolic solution, add 1.500g nanometer grade silica, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 10 with acetic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 48 hours at 220 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 105 DEG C.
Embodiment 8
Get 9ml ethylene glycol and 1ml water is mixed with mixed solution, add 5.200g teos solution, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 8 with citric acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 10 hours at 180 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 90 DEG C.
Embodiment 9
Get 10ml ethylene glycol solution, add 1.500g nanometer grade silica, stir; Add the MnCl of 4.950g 2.4H 2o, stirs; The LiOH of 2.100g is added in the solution of above-mentioned steps preparation, stir; PH value is adjusted to 7.5 with oxalic acid and ethylenediamine, the solution finally preparing is inserted in reactor, solvent thermal reaction 20 hours at 140 DEG C, and water cyclic washing 5 times, alcohol washed twice, filters, and is drying to obtain manganese silicate of lithium material at 150 DEG C.
It is for technical characterstic of the present invention and thinking are described that above example is described, and its object is to allow relevant speciality technical staff can understand content of the present invention and implement accordingly, can not limit the scope of the invention with this.All equivalence changes of doing according to the technology of the present invention feature and thinking or modify, within all should being encompassed in protection scope of the present invention.

Claims (6)

1. a preparation method for manganese silicate of lithium positive electrode for lithium ion battery, concrete steps are as follows:
1) in the mixed solution of organic solvent or organic solvent and water, add manganese salt, lithium salts and nanometer grade silica or tetraethoxysilane as the silicon source of reacting;
2) in step 1) gained solution, add organic acid or organic amine as pH value conditioning agent;
3) by step 2) gained solution carries out solvent thermal reaction, and products therefrom washs, filters, is drying to obtain manganese silicate of lithium material;
Organic solvent in described step 1) is ethanol or ethylene glycol, and the mixed solution of organic solvent and water is the mixed solution of second alcohol and water or the mixed solution of ethylene glycol and water;
The mol ratio of described Mn element, Li element and Si element is: 0.9-1.1:1.8-2.2:0.9-1.1;
The reaction temperature of the solvent thermal reaction in described step 3) is 150～220 DEG C, and the reaction time is 10～48 hours;
Described step 2) the pH value=9-12 of solution of gained.
2. the preparation method of manganese silicate of lithium positive electrode for a kind of lithium ion battery as claimed in claim 1, is characterized in that, in described step 1), manganese salt is one or more the mixture in manganese chloride, manganese acetate, manganese carbonate or manganese sulfate.
3. the preparation method of manganese silicate of lithium positive electrode for a kind of lithium ion battery as claimed in claim 1, is characterized in that, in described step 1), lithium salts is lithium hydroxide.
4. the preparation method of manganese silicate of lithium positive electrode for a kind of lithium ion battery as claimed in claim 1, is characterized in that described step 2) in organic acid be one or more the mixture in formic acid, acetic acid, citric acid or oxalic acid.
5. the preparation method of manganese silicate of lithium positive electrode for a kind of lithium ion battery as claimed in claim 1, is characterized in that described step 2) in organic amine be ethylenediamine.
6. the preparation method of manganese silicate of lithium positive electrode for a kind of lithium ion battery as claimed in claim 1, is characterized in that, in described step 3), baking temperature is 90～150 DEG C.
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CN103545510B (en) * 2013-09-30 2015-12-09 上海维凯光电新材料有限公司 Lithium manganese silicate type positive electrode material of lithium ion battery and preparation method thereof
CN105244498A (en) * 2015-08-31 2016-01-13 无锡市嘉邦电力管道厂 Preparation method for graphene lithium manganese silicate cathode material
CN105845921A (en) * 2016-05-23 2016-08-10 无锡市嘉邦电力管道厂 Preparation method for graphene Li2MnSiO4 positive electrode material
CN105895883B (en) * 2016-06-03 2018-05-29 清华大学深圳研究生院 Complex silicate manganese lithium anode material and preparation method thereof
CN106378139B (en) * 2016-08-26 2019-10-11 北京大学深圳研究生院 A kind of water decomposition catalyst and its preparation method and application
CN106784616B (en) * 2016-12-06 2019-06-25 广州汽车集团股份有限公司 The self-assembly preparation method thereof and positive electrode composition of spherical manganese silicate of lithium composite material

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Patentee after: Suzhou GCL Energy Technology Development Co Ltd

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Patentee before: New materials (Yancheng) Co., Ltd. GCL power