CN104064773A - Preparation method of carbon-coated lithium manganese borate cathode material for lithium ion battery - Google Patents
Preparation method of carbon-coated lithium manganese borate cathode material for lithium ion battery Download PDFInfo
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Abstract
The invention relates to a preparation method of a carbon-coated lithium manganese borate cathode material for a lithium ion battery, belonging to the technical field of lithium ion batteries. The preparation method of the carbon-coated lithium manganese borate cathode material for the lithium ion battery comprises the following process steps of (1) mixing a lithium source compound, a manganese source compound, a boron source compound and a carbon source compound according to the molar ratio that Li to Mn to B to a carbon source is equal to (1-1.05) to 1 to 1 to (0.1-1.0), then, adding deionized water to form a solution, next, continuing to stir at the temperature of 50-90 DEG C to slowly evaporate water to form sol, and then, drying the sol at the temperature of 70-110 DEG C; (2) presintering under the protection of inert gases and at the temperature of 300-400 DEG C for 3-5h, grinding for 5-10min after naturally cooling, flaking at the pressure of 5-20MPa, calcining under the protection of inert gases and at the temperature of 700-850 DEG C for 12-24h, and grinding after naturally cooling to obtain the carbon-coated lithium manganese borate cathode material. The preparation method has the advantages of simple process route, good repeatability, suitability for industrial production and low manufacturing cost; in addition, the prepared material is uniform in particle size distribution, favorable in electrochemical property and the like.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to the preparation method of the coated manganese borate lithium anode material of a kind of lithium ion battery carbon.
Background technology
At present, the chemical property of lithium ion battery depends primarily on electrode material and electrolyte, wherein positive electrode is the part of most critical in lithium ion battery, because it has determined holistic cost, capacity, useful life and the security performance etc. of battery to a great extent.Mainly be divided three classes according to material structure: the one, layer structure material, the 2nd, spinel structure material, the 3rd, polyanion type olivine structural material.
In recent years, the lithium transition-metal borate that contains polyanion receives much concern as Olivine-type Cathode Material in Li-ion Batteries.With LiMnPO
4compare, in structure, substituted phosphate radical with lighter borate, make manganese borate lithium there is higher specific capacity (222mAh/g), and the Conductivity Ratio LiFePO of manganese borate lithium
4high nearly 5 orders of magnitude (B.L.Ellis, W.R.M.Makahnouk, et al., Nature Materials, 2007,6:749.), have obvious advantage, are a kind of anode material for lithium-ion batteries that has very much application prospect.
Solid State Ionics magazine calendar year 2001 has been reported LiMBO
3(M=Fe, Mn, Co) has doff lithium character, can be used as anode material for lithium-ion batteries, but its chemical property is poor.Journal of Alloys and Compounds magazine has been reported by solid phase method at next step synthetic LiMnBO of 850 DEG C of conditions for 2010
3, under 5mA/g current density, discharge capacity is 75.5mAh/g first, and after circulation, each cycle capacity loss is 0.09% first, and along with charging and discharging currents density increases, circulation volume declines, and the discharge capacity first under 50mA/g condition is 42.3mAh/g.For further improving the electric conductivity of manganese borate lithium material, Chinese patent CN102403505A, taking ascorbic acid, humic acid etc. as carbon source, the composite material of the coated manganese borate lithium of synthetic original position carbon, it has higher discharge capacity first and good chemical property, but its cyclical stability still awaits further raising.Chinese patent CN102386418A; make jelly taking boric acid, lithium nitrate, manganese nitrate as predecessor; in follow-up high-temperature heat treatment process; taking the hydrogen-argon-mixed and acetylene of certain volume ratio and the gaseous mixture of argon gas as protective gas; the manganese borate lithium anode material that synthesizing carbon nanotubes is coated; discharge capacity is 185mAh/g first; still nearly 180mAh/g of capacity after 20 circulations; but in this material building-up process, introduce acetylene gas and be the carbon source of preparation carbon nano-tube, cause the problems such as synthetic material consistency of performance is not good enough.
Summary of the invention
The present invention provides the preparation method of the coated manganese borate lithium anode material of a kind of lithium ion battery carbon for solving the technical problem existing in known technology.
The object of this invention is to provide one and have that process route is simple, favorable reproducibility, be applicable to suitability for industrialized production, the cost of raw material and processing cost are low; The manganese borate lithium particle diameter distribution uniform of coating product carbon, and in lithium ion battery, show good chemical property, under 0.1C current density, discharge capacity reaches the preparation method of the coated manganese borate lithium anode material of lithium ion battery carbon of the features such as 83.0mAh/g for the second time.
Lithium ion battery of the present invention by the technical scheme that the preparation method of the coated manganese borate lithium anode material of carbon takes is:
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, is characterized in: the coated manganese borate lithium anode material of carbon comprises following technical process:
(1) first by Li source compound, manganese source compound, boron source compound and carbon-source cpd Li:Mn:B in molar ratio: carbon source=(1～1.05): 1:1:(0.1～1.0) mix, add again deionized water, Li source compound, manganese source compound, boron source compound and carbon-source cpd are dissolved, form solution, continuous stirring under 50～90 DEG C of conditions, make water slow evaporation form colloidal sol, then under 70～110 DEG C of conditions, dry colloidal sol;
(2) pre-burning 3～5h under 300～400 DEG C of inert gas shielding conditions; naturally cooling rear grinding 5～10min at 5～20MPa pressure lower sheeting, calcines 12～24h under 700～850 DEG C of inert gas shielding conditions; naturally cooling rear grinding, makes the coated manganese borate lithium anode material of carbon.
Lithium ion battery of the present invention can also adopt following technical scheme by the preparation method of the coated manganese borate lithium anode material of carbon:
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: the naturally cooling rear milling time of pre-burning 3～5h is 5～10min.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: Li source compound is one or more in two hydration lithium acetates, lithium carbonate, lithium oxalate or lithium citrate.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: manganese source compound is one or more in manganese carbonate, four hydration manganese acetates, manganese oxalate or manganese monoxide.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: boron source compound is four ammonium borate hydrates or boric acid.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: carbon source is one or more in citric acid, adipic acid, glucose, sucrose, lactose, fructose or water soluble starch.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: inert gas is the mist of argon gas, nitrogen, argon gas and hydrogen or the mist of nitrogen and hydrogen.
The preparation method of the coated manganese borate lithium anode material of carbon for described lithium ion battery, is characterized in: in the mist of the mist of argon gas and hydrogen or nitrogen and hydrogen, hydrogen volume content is 2～10%.
Advantage and good effect that the present invention has are:
Lithium ion battery is by the preparation method of the coated manganese borate lithium anode material of carbon owing to having adopted the brand-new technical scheme of the present invention, and compared with prior art, the present invention has following distinguishing feature:
(1) the present invention is dissolved in pre-reaction material in deionized water, wherein taking carbon sources such as citric acids as chelating agent, make colloidal sol in conjunction with thermal evaporation process, compared with solid phase method, colloidal sol is homogeneous phase, and the pre-reaction material being scattered in wherein can reach molecular level mixing, in follow-up high-temperature heat treatment process, can effectively shorten the diffusion distance of ion, thereby make the manganese borate lithium of phase structure homogeneous, the good carbon coated of particle decentralization;
(2) when the carbon source such as citric acid is as chelating agent, can be used as carbon source, high-temperature heat treatment process situ cracking Formed, evenly be coated on the surface of manganese borate lithium material, lysisin situ carbon not only can improve material electric conductivity, and because it has certain reduction characteristic under hot conditions, can prevent that manganese borate lithium is oxidized in high-temperature heat treatment process;
(3) prepare in the process of manganese borate lithium of carbon coated, do not relate to any organic solvent, process environmental protection, safety, have fewer environmental impacts, and material cost and processing cost low, technique is simple, favorable reproducibility, very applicable suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the XRD spectra of the coated manganese borate lithium anode material of the lithium ion battery carbon that makes of the embodiment of the present invention 1;
Fig. 2 is the SEM figure of the coated manganese borate lithium anode material of the lithium ion battery carbon that makes of the embodiment of the present invention 1;
Fig. 3 is the charging and discharging curve figure of the 2nd circulation of the coated manganese borate lithium anode material of the lithium ion battery carbon that makes of the embodiment of the present invention 2.
Embodiment
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
The coated manganese borate lithium of carbon that embodiment of the present invention makes is applied in lithium ion battery, method of testing is: in the manganese borate lithium material powder of carbon coated, add 15wt%Super P carbon black as conductive agent, (PVDF is the PVDF/NMP solution of the 0.02g/mL for preparing to 10wt%PVDF (Kynoar), NMP is 1-METHYLPYRROLIDONE) as binding agent, after stirring, one side is coated on aluminium foil, put into 80 DEG C baking oven dry after, be washed into pole piece with the drift of 12.5 millimeters of diameters, after flattening under the pressure that is 5MPa at pressure, put into the dry 8h of vacuum drying oven of 110 DEG C.Pole piece is transferred in argon gas glove box, taking metal lithium sheet as negative pole, Cellgard2400 is barrier film, the ethylene carbonate of 1.0mol/L lithium hexafluoro phosphate and dimethyl carbonate (volume ratio 1:1) mixed solution is electrolyte, be assembled into CR2016 button cell, on LAND battery test system (Wuhan Jin Nuo Electronics Co., Ltd.), carry out constant current charge-discharge performance test, charging and discharging multiplying power is 0.1C, discharges and recharges cut-ff voltage with respect to Li/Li
+be 1.0～4.8V.
Consult accompanying drawing 1 to Fig. 3.
Embodiment 1
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, its preparation process comprises following processing step:
1. 1.7956g bis-hydration lithium acetates (0.0176 mole of Li), 4.1895g tetra-hydration manganese acetates (0.0171 mole of Mn), 1.0573g boric acid (0.0171 mole of B) and 2.0171g citric acid (0.0105 mole) are mixed, add again appropriate deionized water, two hydration lithium acetates, four hydration manganese acetates, boric acid and citric acid are dissolved, form solution, continuous stirring at 80 DEG C, make water slow evaporation, until then formation colloidal sol dry colloidal sol at 90 DEG C;
2. pre-burning 3h under 350 DEG C of argon shields, naturally cooling rear grinding 10min at the pressure lower sheeting of 10MPa, calcines 12h under 850 DEG C of argon shields, and naturally cooling rear grinding makes the coated manganese borate lithium anode material of carbon.
By the manganese borate lithium of the carbon coated of above-mentioned preparation, on the Ultima IV type X-ray diffractometer of producing in Rigaku group, carry out XRD test.Sweep limits is 10～90 °, 6 °/min of sweep speed.
Fig. 1 is the XRD spectra that embodiment 1 obtains the coated manganese borate lithium anode material of a kind of lithium ion battery carbon, and result shows that material has good hexagonal structure.
Fig. 2 is the SEM figure that embodiment 1 obtains the coated manganese borate lithium anode material of a kind of lithium ion battery carbon, and as seen from the figure, resulting materials is mainly made up of irregular particle, and particle diameter distribution uniform is about 3-5 μ m.
Embodiment 2
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, its preparation process comprises following processing step:
1. 0.7003g lithium oxalate (0.0137 mole of Li), 1.9296g manganese oxalate (0.0135 mole of Mn), 0.8889g tetra-ammonium borate hydrates (0.0135 mole of B) and 2.1081g glucose (0.0117 mole) are mixed, add again appropriate deionized water, lithium oxalate, manganese oxalate, four ammonium borate hydrates and glucose are dissolved, form solution, continuous stirring at 60 DEG C, make water slow evaporation, until then formation colloidal sol dry colloidal sol at 100 DEG C;
2. pre-burning 4h under 300 DEG C of nitrogen protections; naturally cooling rear grinding 5min; at the pressure lower sheeting of 20MPa, in 800 DEG C of argon gas and the lower calcining 24h of hydrogen mixed gas (wherein hydrogen content is 8%) protection, naturally cooling rear grinding makes the coated manganese borate lithium anode material of carbon.
Fig. 3 is the charging and discharging curve figure of the 2nd circulation of the coated manganese borate lithium anode material of a kind of lithium ion battery carbon of obtaining of embodiment 2.As seen from the figure, the cyclic discharge capacity for the second time of the manganese borate lithium of carbon coated is 80mAh/g.
Embodiment 3
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, its preparation process comprises following processing step:
1. 0.6145g lithium carbonate (0.0166 mole of Li), 1.8290g manganese carbonate (0.0159 mole of Mn), 1.0469g tetra-ammonium borate hydrates (0.0159 mole of B) and 1.1846g sucrose (0.0035 mole) are mixed, add again appropriate deionized water, make lithium carbonate, manganese carbonate, four ammonium borate hydrates and sucrose dissolved, form solution, continuous stirring at 90 DEG C, make water slow evaporation, until form colloidal sol, then at 80 DEG C, dry colloidal sol;
2. pre-burning 5h under 350 DEG C of argon shields; naturally cooling rear grinding 10min; at the pressure lower sheeting of 15MPa, in 750 DEG C of nitrogen and the lower calcining 24h of hydrogen mixed gas (hydrogen content is 5%) protection, naturally cooling rear grinding makes the coated manganese borate lithium anode material of carbon.
Embodiment 4
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, its preparation process comprises following processing step:
1. 1.5114g lithium citrate (0.0216 mole of Li), 1.4897g manganese monoxide (0.0210 mole of Mn), 1.2984g boric acid (0.0210 mole of B) and 2.1273g fructose (0.0118 mole) are mixed, add again appropriate deionized water, lithium citrate, manganese monoxide, boric acid and fructose are dissolved, form solution, continuous stirring at 70 DEG C, make water slow evaporation, until form colloidal sol, then at 90 DEG C, dry colloidal sol;
2. pre-burning 3h under 400 DEG C of argon shields, naturally cooling rear grinding 10min at the pressure lower sheeting of 10MPa, calcines 16h under 800 DEG C of inert gas shieldings, and naturally cooling rear grinding makes the coated manganese borate lithium anode material of carbon.
Embodiment 5
A preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, its preparation process comprises following processing step:
1. 0.7003g lithium oxalate (0.0137 mole of Li), 1.9296g manganese oxalate (0.0135 mole of Mn), 0.8889g tetra-ammonium borate hydrates (0.0135 mole of B) and 2.1081g glucose (0.0117 mole) are mixed, add again appropriate deionized water, lithium oxalate, manganese oxalate, four ammonium borate hydrates and glucose are dissolved, form solution, continuous stirring at 50 DEG C, make water slow evaporation, until then formation colloidal sol dry colloidal sol at 110 DEG C;
2. pre-burning 3h under 400 DEG C of nitrogen protections; naturally cooling rear grinding 5min; at the pressure lower sheeting of 20MPa, in 700 DEG C of argon gas and the lower calcining 24h of hydrogen mixed gas (wherein hydrogen content is 10%) protection, naturally cooling rear grinding makes the coated manganese borate lithium anode material of carbon.
The present embodiment has that described process route is simple, favorable reproducibility, is applicable to suitability for industrialized production, and the cost of raw material and processing cost are low; The manganese borate lithium particle diameter distribution uniform of coating product carbon, and in lithium ion battery, show good chemical property, under 0.1C current density, discharge capacity reaches the good effects such as 83.0mAh/g for the second time.
Claims (8)
1. a preparation method for the coated manganese borate lithium anode material of carbon for lithium ion battery, is characterized in that: the coated manganese borate lithium anode material of carbon comprises following technical process:
(1) first by Li source compound, manganese source compound, boron source compound and carbon-source cpd Li:Mn:B in molar ratio: carbon source=(1～1.05): 1:1:(0.1～1.0) mix, add again deionized water, Li source compound, manganese source compound, boron source compound and carbon-source cpd are dissolved, form solution, continuous stirring under 50～90 DEG C of conditions, make water slow evaporation form colloidal sol, then under 70～110 DEG C of conditions, dry colloidal sol;
(2) pre-burning 3～5h under 300～400 DEG C of inert gas shielding conditions; naturally cooling rear grinding at 5～20Mpa pressure lower sheeting, is calcined 12～24h under 700～850 DEG C of inert gas shielding conditions; naturally cooling rear grinding, makes the coated manganese borate lithium anode material of carbon.
2. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1, is characterized in that: the naturally cooling rear milling time of pre-burning 3-5h is 5～10min.
3. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1 and 2, is characterized in that: Li source compound is one or more in two hydration lithium acetates, lithium carbonate, lithium oxalate or lithium citrate.
4. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1 and 2, is characterized in that: manganese source compound is one or more in manganese carbonate, four hydration manganese acetates, manganese oxalate or manganese monoxide.
5. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1 and 2, is characterized in that: boron source compound is four ammonium borate hydrates or boric acid.
6. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1 and 2, is characterized in that: carbon source is one or more in citric acid, adipic acid, glucose, sucrose, lactose, fructose or water soluble starch.
7. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 1 and 2, is characterized in that: inert gas is the mist of argon gas, nitrogen, argon gas and hydrogen or the mist of nitrogen and hydrogen.
8. the preparation method of the coated manganese borate lithium anode material of carbon for lithium ion battery according to claim 7, is characterized in that: in the mist of the mist of argon gas and hydrogen or nitrogen and hydrogen, hydrogen volume content is 2～10%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105609721A (en) * | 2015-12-30 | 2016-05-25 | 中南大学 | Preparation method for three-dimensional carbon net coated lithium manganese borate composite positive electrode material |
| CN108155368A (en) * | 2017-12-29 | 2018-06-12 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods |
| CN110828823A (en) * | 2019-11-19 | 2020-02-21 | 湖北理工学院 | Preparation method of lithium manganese borate/carbon composite material |
| CN113903895A (en) * | 2021-09-27 | 2022-01-07 | 蜂巢能源科技有限公司 | Coating method of cobalt-free positive electrode material, cobalt-free positive electrode material and lithium ion battery |
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| CN102403505A (en) * | 2011-12-15 | 2012-04-04 | 山东大学 | Method for preparing lithium ion battery cathode material in-situ carbon coated lithium manganese borate composite material |
| CN103833044A (en) * | 2014-03-19 | 2014-06-04 | 中南大学 | Preparation method of anode material manganese-lithium borate for lithium ion battery |
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| CN102079530A (en) * | 2009-11-29 | 2011-06-01 | 宁波大学 | Method for preparing lithium iron borate serving as positive material of lithium ion battery by sol-gel technology |
| CN102403505A (en) * | 2011-12-15 | 2012-04-04 | 山东大学 | Method for preparing lithium ion battery cathode material in-situ carbon coated lithium manganese borate composite material |
| CN103833044A (en) * | 2014-03-19 | 2014-06-04 | 中南大学 | Preparation method of anode material manganese-lithium borate for lithium ion battery |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105609721A (en) * | 2015-12-30 | 2016-05-25 | 中南大学 | Preparation method for three-dimensional carbon net coated lithium manganese borate composite positive electrode material |
| CN108155368A (en) * | 2017-12-29 | 2018-06-12 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods |
| CN110828823A (en) * | 2019-11-19 | 2020-02-21 | 湖北理工学院 | Preparation method of lithium manganese borate/carbon composite material |
| CN113903895A (en) * | 2021-09-27 | 2022-01-07 | 蜂巢能源科技有限公司 | Coating method of cobalt-free positive electrode material, cobalt-free positive electrode material and lithium ion battery |
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