CN101807687A - Preparation method of high-performance lithium manganate spinel used for lithium ion battery - Google Patents
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Abstract
The invention relates to a preparation method of high-performance lithium manganate spinel used for a lithium ion battery, which comprises the following steps: (1) raw material selection: selecting power battery-grade electrolytic manganese oxide the grain size of which is 3 to 20 mum and a battery-grade lithium-contained compound the mean grain size of which is not more than 6 mum, wherein the impurity content of the lithium-contained compound is not more than 0.1 percent; (2) preparation environment selection: selecting an environment the height above sea level of which is 1500 to 2500m, the environmental temperature of which is 15 to 40 DEG C and the relative humidity of which is not more than 30 percent; (3) evenly mixing the manganese oxide and the lithium-contained compound in the manganese/lithium molar ratio of 1:0.56-0.58, and then carrying out ball milling and pressing to form a block mixture; and (4) putting the mixture in a continuous sintering furnace for sintering, and then carrying out natural cooling and grading inspection after the reaction is ended to obtain a product Li1+xMn2O4, wherein x is greater than 0 but is less than 0.2. The invention has simple process, and the obtained product has stable quality and good electrochemical properties.
Description
Technical field
The present invention relates to the preparation method of spinel lithium manganate, relate in particular to a kind of preparation method who is used for the high-performance spinel lithium manganate of lithium ion battery.
Background technology
Lithium ion battery because of have the energy density height, have extended cycle life, pollute less, advantage such as memory-less effect, volume are little, in light weight, being used widely in miniature movable type electronic product fields such as mobile phone, notebook computer, electric tools, is the battery that development potentiality is arranged in following electric bicycle, the electric automobile field most.
The commercialization anode material for lithium-ion batteries mainly is cobalt acid lithium (LiCoO at present
2), lithium manganate having spinel structure LiMn
2O
4, nickle cobalt lithium manganate Li (Ni
1/3Co
1/3Mn
1/3) O
2Because rare, the expensive price of cobalt resource, with and toxicity to the influence of environment, cobalt acid lithium thermal stability in the charge and discharge cycles process is on the low side in addition, so cobalt is that the large-scale application development potentiality of sour lithium must be restricted; Comparatively speaking, lithium manganate having spinel structure is because the close friend of cheap, the environment of abundant, the price of manganese resource, have simultaneously high-rate charge-discharge capability, thermal stability and security performance preferably again, therefore, LiMn2O4 is as anode material for lithium-ion batteries, and especially the application in high power lithium batteries such as electric tool, electric motor car is very promising.
Yet, traditional LiMn2O4 is in long charge and discharge cycles process, particularly under the high temperature charge and discharge cycles, dissolving because of manganese, cause cycle performance of battery obviously to descend, Jahn-Teller malformation easily takes place when discharge off in addition, and these factors have all reduced high temperature cyclic performance, cycle performance and the big current work performance of battery.Improved cycle performance though can reduce the dissolving of manganese to a certain extent by methods such as doping, surface coatings, but because the adding of inert matter, tend to sacrifice energy content of battery density, make that simultaneously complicated process of preparationization, the common impurity element of introducing mainly are that Co, Ni etc. also can cause environmental pollution and cost to increase.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, the preparation method of the high-performance spinel lithium manganate that is used for lithium ion battery of constant product quality.
For addressing the above problem, a kind of preparation method who is used for the high-performance spinel lithium manganate of lithium ion battery of the present invention may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56～0.58 after, through ball milling, be pressed into block mixture;
(4) mixture of described step (3) gained is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5～2h, heated at constant temperature 6～10h under 560～600 ℃ of temperature, heated at constant temperature 12～24h under 730～810 ℃ of temperature at last then under 100～200 ℃ of temperature; After the roasting reaction is finished, natural cooling 10～30h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
Manganese oxide in the described step (1) is any one in manganese dioxide, manganese sesquioxide managnic oxide, the mangano-manganic oxide.
Lithium-containing compound in the described step (1) is lithium carbonate or lithium hydroxide.
The present invention compared with prior art has the following advantages:
1, the present invention is by the improvement to technological principle such as raw material, manganese/lithium molar ratio, roast process and process conditions, reduced the moisture in the spinel lithium manganate effectively, reduce the spinel lithium manganate crystal defect, thereby promoted the structural stability of lithium manganate having spinel structure, reduce the manganese dissolving in long circulation and high temperature circulation process, thereby improved the cycle performance of battery.
2, the present invention is by improving the content of lithium in the lithium manganese oxide, and making the product that finally obtains is the LiMn2O4 Li of rich lithium
1+xMn
2O
4(0＜x＜0.2).
(1) the LiMn2O4 sample that adopts the present invention's preparation carries out micro-structural characterization test (testing conditions: after testing sample placed diffractometer sample stage position with X-Ray polycrystal powder diffractometer, gathering diffraction with the step scanning mode composes entirely, rank are wide: 0.02 °, and per step time of staying 2S, 2
Scope: 10～80 °.), can find that the product of gained of the present invention meets the diffracting spectrum of spinel lithium manganate, have perfect spinel structure, there is not dephasign to have (referring to Fig. 1) in the product structure.
(2) adopt the LiMn2O4 sample of the present invention's preparation to carry out microscopic appearance characterization test (testing conditions: accelerating voltage 10KV, operating distance 5mm, enlargement ratio 10000 with scanning electron microscopy.), can find that the product of gained of the present invention has the characteristics that particle size distribution is even, crystalline structure is complete (referring to Fig. 2).
(3) the LiMn2O4 sample with the present invention's preparation is that positive electrode, graphite are negative material, with conductive agent carbon black (3wt%), binding agent Kynoar (PVDF, N-methyl pyrrolidone (NMP) solution 3wt%) and above-mentioned positive electrode active materials LiMn
2O
4(94wt%) mix, make slurry, be coated in the two-sided positive plate that makes of aluminium foil, being assembled into model by ordinary production technology is 053048 battery, electrolyte uses vinyl carbonate (EC)/dimethyl carbonate (DMC) (volume ratio of the two is 1: 1) of the LiPF6 of 1 mol, its charge-discharge performance of test on cell tester, test shows that the product of gained of the present invention has the characteristics (referring to table 1) that have extended cycle life.
Table 1: charge-discharge performance test chart
| Sample number into spectrum | Initial specific capacity | 1C 300 capability retentions (25 ℃) that circulate | 1C 500 capability retentions (25 ℃) that circulate | 1C 300 capability retentions (55 ℃) that circulate | 5C 300 capability retentions (25 ℃) that circulate | 5C 300 capability retentions (55 ℃) that circulate |
| Comparative Examples 1 | ??93 | ??≥80 | ??≥65 | ??≥62 | ??≥73 | ??≥58 |
| Embodiment 1 | ??95 | ??≥93 | ??≥86 | ??≥81 | ??≥90 | ??≥79 |
| Embodiment 2 | ??94 | ??≥94 | ??≥88 | ??≥83 | ??≥92 | ??≥81 |
| Embodiment 3 | ??93 | ??≥95 | ??≥89 | ??≥85 | ??≥94 | ??≥82 |
| Embodiment 4 | ??98 | ??≥92 | ??≥85 | ??≥80 | ??≥89 | ??≥79 |
(4) high-multiplying power discharge characteristic, high temperature cyclic performance and low self-discharge rate.
As can be found from Table 1, circulate 300 capability retentions greater than 80% at 55 ℃ of following 1C; 300 capability retentions of 5C circulation at normal temperatures circulate 300 capability retentions greater than 79% greater than 88%, 55 ℃ of following 5C.The product of gained of the present invention has high temperature cyclic performance and high-rate discharge ability.
Battery was placed 30 days at normal temperatures, and capability retention is 97%; Battery was at high temperature placed 7 days, and capability retention is greater than 90%.The product of gained of the present invention has the low self-discharge rate.
In sum, the LiMn2O4 Li of the rich lithium of gained of the present invention
1+xMn
2O
4(0＜x＜0.2) has excellent electrochemical properties, not only overcome the shortcoming of traditional lithium manganate having spinel structure cycle life weak point, high-temperature behavior difference, and be adapted to the requirement of heavy-current discharge, and improve than multiplying power discharging characteristic, especially be fit to the discharge characteristics of electric vehicle electrokinetic cell.
3, because the present invention only adopts manganese oxide and lithium-containing compound as raw material, and these two kinds of raw materials itself do not contain any harmful element, and therefore, the present invention can not pollute environment.
4, because operating process of the present invention is relatively independent, simple, can control various piece respectively, therefore, technology plasticity is strong, can change product by adjustment raw material, roast technology, meets the different needs.
5, because artifical influence factor of the present invention is few, can carry out strictness to technical process and monitor, therefore, guarantee the consistency of technical process, thereby made the constant product quality of gained of the present invention.
6, technology of the present invention simple, with low cost, be easy to large-scale production.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Fig. 1 is the diffracting spectrum of LiMn2O4 sample among the present invention.
Fig. 2 is the electronic scanning figure of LiMn2O4 sample among the present invention.
Embodiment
The preparation method of Comparative Examples 1 spinel lithium manganate may further comprise the steps:
(1) material choice: selecting particle diameter is the electrokinetic cell level electrolytic oxidation manganese of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%.
Wherein: manganese oxide is a manganese dioxide, and lithium-containing compound is a lithium carbonate.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity 60%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5h, heated at constant temperature 8h under 580 ℃ of temperature, heated at constant temperature 16h under 760 ℃ of temperature at last then under 100 ℃ of temperature; After the roasting reaction is finished, natural cooling 20h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
1 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a manganese dioxide, and lithium-containing compound is a lithium carbonate.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5h, heated at constant temperature 8h under 580 ℃ of temperature, heated at constant temperature 16h under 760 ℃ of temperature at last then under 100 ℃ of temperature; After the roasting reaction is finished, natural cooling 20h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
2 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a manganese sesquioxide managnic oxide; Lithium-containing compound is a lithium carbonate.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.58 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5h, heated at constant temperature 8h under 580 ℃ of temperature, heated at constant temperature 16h under 760 ℃ of temperature at last then under 100 ℃ of temperature; After the roasting reaction is finished, natural cooling 20h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
3 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a mangano-manganic oxide, and lithium-containing compound is a lithium hydroxide.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 1h, heated at constant temperature 6h under 600 ℃ of temperature, heated at constant temperature 12h under 810 ℃ of temperature at last then under 150 ℃ of temperature; After the roasting reaction is finished, natural cooling 25h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
4 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a manganese dioxide, and lithium-containing compound is a lithium hydroxide.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 1.5h, heated at constant temperature 10h under 560 ℃ of temperature, heated at constant temperature 20h under 730 ℃ of temperature at last then under 200 ℃ of temperature; After the roasting reaction is finished, natural cooling 15h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
5 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a manganese sesquioxide managnic oxide, and lithium-containing compound is a lithium hydroxide.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.57 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 2h, heated at constant temperature 8h under 580 ℃ of temperature, heated at constant temperature 24h under 730 ℃ of temperature at last then under 150 ℃ of temperature; After the roasting reaction is finished, natural cooling 10h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
6 one kinds of preparation methods that are used for the high-performance spinel lithium manganate of lithium ion battery of embodiment may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
Wherein: manganese oxide is a mangano-manganic oxide, and lithium-containing compound is a lithium hydroxide.
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.57 after, through ball milling, be pressed into block mixture;
(4) mixture is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5h, heated at constant temperature 8h under 580 ℃ of temperature, heated at constant temperature 12h under 800 ℃ of temperature at last then under 100 ℃ of temperature; After the roasting reaction is finished, natural cooling 30h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
Claims (3)
1. preparation method who is used for the high-performance spinel lithium manganate of lithium ion battery may further comprise the steps:
(1) material choice: selecting particle diameter is the electrolytic oxidation manganese of the electrokinetic cell level of 3～20um; The LITHIUM BATTERY lithium-containing compound of average grain diameter≤6um, its impurity content≤0.1%;
(2) preparation environmental selection: selecting height above sea level is 1500～2500 meters, and ambient temperature is 15～40 ℃, the environment of relative humidity≤30%;
(3) manganese oxide and lithium-containing compound are evenly mixed by manganese/lithium mol ratio of 1: 0.56～0.58 after, through ball milling, be pressed into block mixture;
(4) mixture of described step (3) gained is gone in the continous way sintering furnace, earlier heated at constant temperature 0.5～2h, heated at constant temperature 6～10h under 560～600 ℃ of temperature, heated at constant temperature 12～24h under 730～810 ℃ of temperature at last then under 100～200 ℃ of temperature; After the roasting reaction is finished, natural cooling 10～30h in the continous way sintering furnace, hierarchical verification promptly obtains product Li
1+xMn
2O
4, 0＜x＜0.2 wherein.
2. a kind of preparation method who is used for the high-performance spinel lithium manganate of lithium ion battery as claimed in claim 1 is characterized in that: the manganese oxide in the described step (1) is any one in manganese dioxide, manganese sesquioxide managnic oxide, the mangano-manganic oxide.
3. a kind of preparation method who is used for the high-performance spinel lithium manganate of lithium ion battery as claimed in claim 1, it is characterized in that: the lithium-containing compound in the described step (1) is lithium carbonate or lithium hydroxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336441A (en) * | 2011-06-29 | 2012-02-01 | 金瑞新材料科技股份有限公司 | Method for preparing lithium manganate used as lithium ion battery anode material by using trimanganese tetroxide |
| CN102751482A (en) * | 2012-07-03 | 2012-10-24 | 四川大学 | High-performance lithium manganate anode material and preparation method thereof |
| CN104600281A (en) * | 2014-12-30 | 2015-05-06 | 山东神工海特电子科技有限公司 | Preparation method of lithium manganate material and method for preparing battery from lithium manganate material |
| CN114085069A (en) * | 2021-11-17 | 2022-02-25 | 柳州紫荆循环能源科技有限公司 | Lithium manganate cathode target material for preparing thin film lithium battery and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336441A (en) * | 2011-06-29 | 2012-02-01 | 金瑞新材料科技股份有限公司 | Method for preparing lithium manganate used as lithium ion battery anode material by using trimanganese tetroxide |
| CN102336441B (en) * | 2011-06-29 | 2013-07-03 | 金瑞新材料科技股份有限公司 | Method for preparing lithium manganate used as lithium ion battery anode material by using trimanganese tetroxide |
| CN102751482A (en) * | 2012-07-03 | 2012-10-24 | 四川大学 | High-performance lithium manganate anode material and preparation method thereof |
| CN102751482B (en) * | 2012-07-03 | 2014-12-03 | 四川大学 | High-performance lithium manganate anode material and preparation method thereof |
| CN104600281A (en) * | 2014-12-30 | 2015-05-06 | 山东神工海特电子科技有限公司 | Preparation method of lithium manganate material and method for preparing battery from lithium manganate material |
| CN114085069A (en) * | 2021-11-17 | 2022-02-25 | 柳州紫荆循环能源科技有限公司 | Lithium manganate cathode target material for preparing thin film lithium battery and preparation method thereof |
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