CN102299315A - Preparation method of lithium manganate anode material - Google Patents
Preparation method of lithium manganate anode material Download PDFInfo
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- CN102299315A CN102299315A CN2011102025048A CN201110202504A CN102299315A CN 102299315 A CN102299315 A CN 102299315A CN 2011102025048 A CN2011102025048 A CN 2011102025048A CN 201110202504 A CN201110202504 A CN 201110202504A CN 102299315 A CN102299315 A CN 102299315A
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- lithium
- lithium manganate
- preparation
- anode material
- cathode material
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Abstract
The invention provides a preparation method of a lithium manganate anode material. The preparation method comprises the following steps of mixing uniformly lithium carbonate, manganese dioxide and at least one doping agent according to a ratio of Li ions to Mn ions to doped ions, wherein the ratio is (0.5 to 0.65): (1 to 1.2): (0.01 to 0.02), putting the mixture into a crucible, putting the crucible containing the mixture into a microwave sintering furnace to sinter for 8 hours at the power of 3kW, maintaining for 8 hours at the power of 800W to obtain uniform lithium manganate with good crystallinity, washing the obtained lithium manganate, filtering, drying by an oven, and sieving by a sieve of 200 meshes to obtain the lithium manganate anode material. The lithium manganate anode material prepared by the preparation method overcomes the defect that based on a solid phase method, materials cannot be heated evenly in synthesis. The lithium manganate anode material has good crystallinity of lithium manganate and realizes improvement of cycle performances and capacity of lithium manganate. In the invention, through microwave sintering, sintering time is reduced greatly; an electric power resource is saved greatly; and a purpose of energy saving and emission reduction is realized.
Description
Technical field
The present invention relates to the preparation method of a kind of method for preparing anode material of lithium-ion battery, particularly a kind of manganate cathode material for lithium.
Background technology
In lithium ion battery, positive electrode is its most important component, also is the key of decision lithium ion battery performance.Spinel-type LiMn
2O
4Be in recent years by one of lithium ion utmost point material of extensive concern, with present commerce positive electrode LiCoO
2Compare have aboundresources, advantage such as cheap, nontoxic pollution-free, the agent structure of spinel lithium manganate is done cube tightly packed composition of rule by oxonium ion, lithium ion and manganese ion occupy respectively in tetrahedron and octahedral interstices, and its simplest formula is LiMn
2O
4, the sky with Fd3m (No.227) is asked the group, lithium ion is distributed in the manganese oxygen octahedra 3 D pore canal on every side, thereby guarantees its migration in the duct, makes charge and discharge process have excellent cycle performance.
Spinel-type LiMn
2O
4Embedding with respect to lithium metal. deviate from current potential about 4V, with LiCoO
2And LiNiO
2Approaching.The ABUNDANT NATUREAL RESOURSES of manganese can keep low-cost in a large amount of uses of lithium ion battery.And the history that manganese compound uses in battery industry is very long, and experienced to the processing of manganese compound and recovery can not caused very big pollution to environment.
Studies show that synthetic method has significant effects to product structure and performance, therefore, develop new method and prepare spinel-type LiMn
2O
4Material becomes one of important channel of improving its performance.Be commonly used to prepare LiMn at present
2O
4Method be mainly conventional solid-state method, the method simple and fast, but batch mixing inequality, raw material is heated inhomogeneous, thing phase purity is limited to, and power consumption is huge, the cost greater energy consumption is big, properties of product are relatively poor.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of manganate cathode material for lithium, solved solid phase method synthetic in the material uneven drawback of being heated, obtain the LiMn2O4 of better crystallinity degree, improved the cycle performance and the capacity of LiMn2O4.
For solving above technical problem, the invention provides a kind of preparation method of manganate cathode material for lithium, with lithium carbonate, manganese dioxide and dopant with Li: Mn: dopant ion is (0.5～0.65): (1 :～1.2): after the ratio of (0.01～0.02) is evenly mixed, place crucible, in microwave agglomerating furnace, heat 8h with 3kW, keep 8h with 800W again, obtain the uniform mutually LiMn2O4 of better crystallinity degree, thing, after at last 200 mesh sieves being crossed in resulting LiMn2O4 washing, filtration, oven dry back, promptly get manganate cathode material for lithium.
As most preferred embodiment of the present invention, described dopant is selected from MgCO
3, TiO
2, Cr
2O
3, Al
2O
3, Co
2O
3, V
2O
5And in the rare earth oxide one or more;
As most preferred embodiment of the present invention, described Li: Mn: dopant ion is (0.5～0.6): (1 :～1.1): (0.01～0.015);
As most preferred embodiment of the present invention, described Li: Mn: dopant ion is (0.6～0.65): (1.1 :～1.2): (0.015～0.02);
As most preferred embodiment of the present invention, described bake out temperature is 150 ℃.
Compared with prior art, the preparation method of manganate cathode material for lithium of the present invention has the following advantages at least: the present invention compares with conventional solid-state method by the LiFePO4 that the microwave sintering method obtains, the product particle is uniformity more, and degree of crystallinity is better, has promoted product quality.Help the stable LiMn2O4 of processability, and can save the energy, shorten the production cycle, enhance productivity.
Description of drawings
Fig. 1 is the XRD figure of the LiMn2O4 that microwave synthesizes in the embodiment of the invention 1;
Fig. 2 is the SEM pattern picture of the LiMn2O4 that microwave synthesizes in the embodiment of the invention 1.
Embodiment
Preparation method to manganate cathode material for lithium of the present invention is described in detail below in conjunction with accompanying drawing:
Embodiment 1
1) with lithium carbonate, manganese dioxide, magnesium carbonate according to Li: Mn: Mg=0.6: 1.1: 0.015 mol ratio is evenly mixed,
2) above-mentioned mixed raw materials is packed in the crucible, place in the microwave agglomerating furnace,, keep 8h with 800W again, promptly get the uniform mutually LiMn2O4 of better crystallinity degree, thing with 3kW heating 8h.
3) above-mentioned gained LiMn2O4 sample is washed three times through pure water, and filter,, and then cross 200 mesh sieves, obtain colory manganate cathode material for lithium through 150 ℃ of oven dry.
The XRD figure of the sample that present embodiment 1 obtains as shown in Figure 1, thing is mutually very pure, degree of crystallinity is also fine, its pattern is as shown in Figure 2.
1) with lithium carbonate, manganese dioxide, magnesium carbonate according to Li: Mn: Mg=0.5: 1: 0.01 mol ratio is evenly mixed,
2) above-mentioned mixed raw materials is packed in the crucible, place in the microwave agglomerating furnace,, keep 8h with 800W again, promptly get the uniform mutually LiMn2O4 of better crystallinity degree, thing with 3kW heating 8h.
3) above-mentioned gained LiMn2O4 sample is washed three times through pure water, and filter,, and then cross 200 mesh sieves, obtain colory manganate cathode material for lithium through 150 ℃ of oven dry.
Embodiment 3
1) with lithium carbonate, manganese dioxide, magnesium carbonate according to Li: Mn: Mg=0.65: 1.2: 0.02 mol ratio is evenly mixed,
2) above-mentioned mixed raw materials is packed in the crucible, place in the microwave agglomerating furnace,, keep 8h with 800W again, promptly get the uniform mutually LiMn2O4 of better crystallinity degree, thing with 3kW heating 8h.
3) above-mentioned gained LiMn2O4 sample is washed three times through pure water, and filter,, and then cross 200 mesh sieves, obtain colory manganate cathode material for lithium through 150 ℃ of oven dry.
The above is a kind of execution mode for inventing only, it or not whole or unique execution mode, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification of the present invention is claim of the present invention and contains.
Claims (5)
1. the preparation method of a manganate cathode material for lithium, it is characterized in that: with lithium carbonate, manganese dioxide and dopant with Li: Mn: dopant ion is (0.5～0.65): (1 :～1.2): after the ratio of (0.01～0.02) is evenly mixed, place crucible, in microwave agglomerating furnace, heat 8h with 3kW, keep 8h with 800W again, obtain better crystallinity degree, thing uniform LiMn2O4 mutually, at last with resulting LiMn2O4 washing, filter, after the oven dry back crosses 200 mesh sieves, promptly get manganate cathode material for lithium.
2. the preparation method of manganate cathode material for lithium as claimed in claim 1, it is characterized in that: described dopant is selected from MgCO
3, TiO
2, Cr
2O
3, Al
2O
3, Co
2O
3, V
2O
5And in the rare earth oxide one or more.
3. the preparation method of manganate cathode material for lithium as claimed in claim 1 or 2 is characterized in that: described Li: Mn: dopant ion is (0.5～0.6): (1 :～1.1): (0.01～0.015).
4. the preparation method of manganate cathode material for lithium as claimed in claim 1 or 2 is characterized in that: described Li: Mn: dopant ion is (0.6～0.65): (1.1 :～1.2): (0.015～0.02).
5. the preparation method of manganate cathode material for lithium as claimed in claim 1, it is characterized in that: described bake out temperature is 150 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400976A (en) * | 2013-08-16 | 2013-11-20 | 深圳市德方纳米科技有限公司 | Titanium nitride coated lithium titanate material preparation method |
| CN104466165A (en) * | 2014-12-11 | 2015-03-25 | 中信大锰矿业有限责任公司大新锰矿分公司 | Modified lithium manganate positive pole material and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101459239A (en) * | 2007-12-14 | 2009-06-17 | 中国电子科技集团公司第十八研究所 | Preparation for lithium battery anode active material |
| CN101800309A (en) * | 2010-04-16 | 2010-08-11 | 中国科学院新疆理化技术研究所 | Microwave synthesis method for multi-element lithium manganate-doped positive electrode material of lithium ion battery |
| CN101913655A (en) * | 2010-09-10 | 2010-12-15 | 河南联合新能源有限公司 | Method for preparing lithium manganate cathode material by microwave sintering |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101459239A (en) * | 2007-12-14 | 2009-06-17 | 中国电子科技集团公司第十八研究所 | Preparation for lithium battery anode active material |
| CN101800309A (en) * | 2010-04-16 | 2010-08-11 | 中国科学院新疆理化技术研究所 | Microwave synthesis method for multi-element lithium manganate-doped positive electrode material of lithium ion battery |
| CN101913655A (en) * | 2010-09-10 | 2010-12-15 | 河南联合新能源有限公司 | Method for preparing lithium manganate cathode material by microwave sintering |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400976A (en) * | 2013-08-16 | 2013-11-20 | 深圳市德方纳米科技有限公司 | Titanium nitride coated lithium titanate material preparation method |
| CN104466165A (en) * | 2014-12-11 | 2015-03-25 | 中信大锰矿业有限责任公司大新锰矿分公司 | Modified lithium manganate positive pole material and preparation method |
| CN104466165B (en) * | 2014-12-11 | 2016-09-28 | 中信大锰矿业有限责任公司大新锰矿分公司 | A kind of modified lithium manganate cathode material and preparation method |
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Application publication date: 20111228 |