CN105789568A - Sulfur element doped lithium-rich lithium manganese oxide material and preparation method thereof - Google Patents
Sulfur element doped lithium-rich lithium manganese oxide material and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a positive electrode material of a lithium ion battery and a preparation method thereof, and specifically relates to a sulfur element doped lithium-rich lithium manganese oxide material and a preparation method thereof. A general formula of the sulfur element doped lithium-rich lithium manganese oxide material is Li<1.2>M<x>Mn<2-x>O<4-y>S<y>, wherein x is greater than or equal to 0.2 and less than 0, and y is greater than or equal to 0.2 and less than 0. Doped positive ions and sulfur atoms are uniformly doped in a lattice of a lithium manganese oxide material according to a certain proportion by using a sol-gel method and a chelator, so that a Jahn-Teller effect of the lithium manganese oxide material is effectively inhibited, a defect of low specific capacity of the lithium manganese oxide caused by the fact that existing spinel lithium manganese oxide can use only a capacity of a 4V area is overcome, the sulfur element doped lithium-rich lithium manganese oxide material can use capacities of both the 4V area and a 3V area, and the discharge specific capacity of the sulfur element doped lithium-rich lithium manganese oxide material is greater than 180mAh/g. The sulfur element doped lithium-rich lithium manganese oxide material can be used as the positive electrode material of small or large lithium ion batteries.
Description
Technical field
The present invention relates to a kind of lithium manganate material and preparation method thereof, particularly relate to a kind of doping element sulphur richness lithium lithium manganate material being applied to anode material for lithium-ion batteries and preparation method thereof.
Background technology
Lithium ion battery, as a kind of novel battery, has the plurality of advantages such as voltage is high, lightweight, volume is little, self discharge is few, is therefore widely used in the fields such as portable electrical appliance, such as mobile phone, notebook computer, digital product etc..Cobalt acid lithium material is simple due to its preparation method, stability of material is good, the factors such as manufacturing process is ripe become the anode material for lithium-ion batteries that consumption on market is more, but cobalt resource is deficient, material price is expensive, and cobalt has important application on electronic applications and military affairs, belongs to strategic resources, therefore its application receives certain restriction.
Lithium manganate having spinel structure has the advantages such as raw material resources are abundant, cheap, safety is good, non-environmental-pollution, easy preparation, it is believed that be one of positive electrode most with development and application prospect；Especially its outstanding security performance and price advantage, become the preferred material of lithium ion battery for electric vehicle positive electrode.But lithium manganate material still suffers from two than more serious shortcoming: one is that lithium manganate material is currently available that specific capacity little (about 110mAh/g)；Two is that it exists comparatively serious capacity fade problem.
For the capacity fade problem of lithium manganate material, current research thinks that caused by the dissolving mainly due to Jahn-Teller effect and manganese, therefore the discharge voltage of manganate cathode material for lithium can not be too low, otherwise may result in the cycle performance of material and worsens.Research shows, the preparation method of lithium manganate having spinel structure material and structure composition are very big to its Electrochemical Performances.The good spinel-type positive electrode of chemical property can be synthesized by method of modifying such as suitable ion doping, Surface coating.Solving lithium manganate having spinel structure capacity fade problem at present adopts maximum methods to be cation doping, the cycle performance aspect improving lithium manganate having spinel structure is had been achieved for good result by the method for cation doping, but it is disadvantageous in that the cation of doping replaces the position of Mn, reduces the initial capacity of material.Additionally, current research focuses primarily upon the 4V district current potential of LiMn2O4, it is greatly reduced charge and discharge voltage range, causes that the capacity in the 3V district of LiMn2O4 cannot utilize, have impact on the actual capacity of material.
Summary of the invention
Rich lithium lithium manganate material that it is an object of the invention to provide a kind of element sulphur that adulterates and preparation method thereof.This material is used as anode material for lithium-ion batteries, there is high power capacity and long-life feature, overcome current lithium manganate having spinel structure only with the capacity in 4V district thus the shortcoming causing its specific capacity relatively low, the material of the present invention can give play to the capacity in its 4V district and 3V district simultaneously, and therefore its specific capacity is generally higher than 180mAh/g.This material can serve as small-sized and large-scale anode material for lithium-ion batteries.
For solving above-mentioned technical problem, technical scheme is as follows:
A kind of manganate cathode material for lithium, it is characterised in that the formula of described manganate cathode material for lithium is Li1.2MxMn2-xO4-ySy, wherein 0 >=x >=0.2,0 >=y >=0.2.
Described doped chemical M is one or more in Li, Na, K, Mg, Ca, Sr, Ba, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Ag, Ce, Sm, Eu, Al, Si, In, Ga, Ge, Sn, Pb, B, Sb, Bi, Se, Te.
The preparation method of a kind of lithium manganate material, comprises the steps:
(1) adopting kipp gas generator principle by dilute sulfuric acid and Iron sulfuret. hybrid reaction generation hydrogen sulfide gas, passed into by the gas of generation and generate Manganese monosulfide. precipitation in manganese salt solution, then filtration, washing, drying obtain Manganese monosulfide. pressed powder；
(2) a kind of polynary organic monoacid is proportionally added in a kind of polyhydric alcohol and forms mixed solution；
(3) by lithium salts, manganese salt and additive are dissolved in above-mentioned mixed solution according to a certain percentage, polynary organic monoacid forms chelate with lithium ion and manganese ion, whole system is uniform solution, now Manganese monosulfide. pressed powder is scattered in solution, and stir, after ultrasonic disperse, heated solution at 60 90 DEG C of temperature, this chelate and polyhydric alcohol generation esterification, solution becomes colloidal sol, continue to add thermosol and remove unnecessary alcohol to obtain gel, add further and be thermally generated xerogel, by xerogel in Muffle furnace at 400 DEG C isothermal holding 3 10 hours, grind tabletting after being cooled to room temperature and obtain presoma；
(4) it is placed in stove at 750 DEG C of temperature by the presoma obtained in step (3) heat treatment 3-15 hour, is cooled to 600 DEG C subsequently and is incubated 3-10 hour, be subsequently cooled to room temperature, pulverize and obtain described manganate cathode material for lithium.
Described manganese salt be manganese sulfate, manganese chloride, manganese nitrate, manganese acetate one or more.
Described polynary organic monoacid be citric acid, oxalic acid, tartaric acid, benzoic acid, salicylic one or more.
Described polyhydric alcohol is ethylene glycol, 1,2 propylene glycol, Isosorbide-5-Nitrae fourth two. alcohol, hexanediol, neopentyl glycol, Diethylene Glycol, dipropylene glycol, trimethylolpropane, glycerol one or more.
Principles of the invention is: lithium manganate having spinel structure positive electrode in charge and discharge process, Li+Spinel structure reversibly embeds, and in 0≤x≤1 and 1≤x≤2 scope, forms two discharge platforms of 3V and 4V respectively, at 4V district Li+Entering the tetrahedron 8a position of spinel structure, in charge and discharge process, capacity attenuation is slower.But at 3V district, Li+Entering the octahedra 16c position in spinel structure, cause strong Jahn Teller to distort, capacity is decayed rapidly.Therefore lithium manganate having spinel structure positive electrode is generally limited to the operated within range of about 4V, and its theoretical capacity also only has 148mAh/g.If lithium manganate having spinel structure positive electrode can overcome the Jahn Teller in 3V district to distort, enable the material to use in two regions of 3V and 4V, then the theoretical capacity of this material nearly doubles.Theoretical Calculation adopts anion doped lithium manganate having spinel structure positive electrode can suppress Jahn Teller effect with experiments show that.
The present invention has an advantage that
(1) element sulphur mix the Jahn Teller effect inhibiting material in 3V district, reduce material dissolving in the electrolyte simultaneously.
(2) element sulphur coordinates other cationic doping, makes the lithium manganate material can at bigger charge and discharge voltage operated within range, and the capacity of material is greatly improved, and the cycle performance of material have also been obtained and greatly improves simultaneously.
(3) preparation method of material is simple, it is easy to operation and control, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of present invention manganate cathode material for lithium obtained by embodiment 1.
Fig. 2 is the XRD figure of present invention manganate cathode material for lithium obtained by embodiment 1.
Fig. 3 is the charging and discharging curve figure of present invention manganate cathode material for lithium obtained by embodiment 1.
Detailed description of the invention
Be will assist in by following embodiment and accompanying drawing and understand the present invention, but be not intended to present disclosure.
Embodiment 1
A kind of lithium manganate material is Li1.2Al0.1Mn1.9O3.96S0.04, its preparation method is as follows:
(1) adopting kipp gas generator by dilute sulfuric acid and Iron sulfuret. hybrid reaction generation hydrogen sulfide gas, passed into by the gas of generation and generate Manganese monosulfide. precipitation in manganese acetate solution, then filtration, washing, drying obtain Manganese monosulfide. pressed powder, standby；
(2) by Li:Al: Mn: S molar ratio is standby for weighing a certain amount of lithium nitrate, aluminum nitrate, manganese acetate, Manganese monosulfide. by 1.2:0.1: 1.9: 0.04；
(3) weigh citric acid in proportion and hexanediol is configured to mixed solution；
(4) lithium nitrate weighed in step (2), aluminum nitrate and manganese acetate are dissolved in deionized water respectively, add after mix homogeneously in the mixed solution of step (3)；This mixed solution is heated under continuous strong stirring, and Manganese monosulfide. powder load weighted in step (2) is diffused slowly in this mixed solution, being incubated a period of time when temperature is increased to 80 DEG C, until mixed liquor becomes gel, further heat drying becomes xerogel；
(5) xerogel is transferred to 400 DEG C of heat treatments of constant temperature 3 hours in Muffle furnace, it is cooled to room temperature with furnace temperature, 750 DEG C of heat treatments of constant temperature 10 hours in Muffle furnace are placed into after grinding tabletting, it is cooled to 600 DEG C of heat treatments subsequently 8 hours, pulverizes after naturally cooling to room temperature and namely obtain described manganate cathode material for lithium.
Embodiment 2
A kind of lithium manganate material is Li1.2Co0.1Mn1.9O3.98S0.02, its preparation method is as follows:
(1) a certain amount of sodium sulfide and manganese acetate are weighed in proportion, respectively sodium sulfide and manganese acetate are configured to aqueous solution, being instilled lentamente by manganese acetate solution and generate Manganese monosulfide. precipitation in sodium sulfide solution, then filtration, washing, drying obtain Manganese monosulfide. pressed powder, standby；
(2) by Li:Co: Mn: S molar ratio is standby for weighing a certain amount of lithium nitrate, cobalt acetate, manganese acetate, Manganese monosulfide. by 1.2:0.1: 1.9: 0.02；
(3) weigh citric acid in proportion and hexanediol is configured to mixed solution；
(4) lithium nitrate weighed in step (2), aluminum nitrate and manganese acetate are dissolved in deionized water respectively, add after mix homogeneously in the mixed solution of step (3)；This mixed solution is heated under continuous strong stirring, and Manganese monosulfide. powder load weighted in step (2) is diffused slowly in this mixed solution, being incubated a period of time when temperature is increased to 80 DEG C, until mixed liquor becomes gel, further heat drying becomes xerogel；
(5) xerogel is transferred to 400 DEG C of heat treatments of constant temperature 3 hours in Muffle furnace, it is cooled to room temperature with furnace temperature, 750 DEG C of heat treatments of constant temperature 10 hours in Muffle furnace are placed into after grinding tabletting, it is cooled to 600 DEG C of heat treatments subsequently 8 hours, pulverizes after naturally cooling to room temperature and namely obtain described manganate cathode material for lithium.
Embodiment 3
A kind of lithium manganate material is Li1.2Cr0.1Mn1.9O3.97S0.03, its preparation method is as follows:
(1) adopting kipp gas generator principle by dilute sulfuric acid and Iron sulfuret. hybrid reaction generation hydrogen sulfide gas, passed into by the gas of generation and generate Manganese monosulfide. precipitation in manganese acetate solution, then filtration, washing, drying obtain Manganese monosulfide. pressed powder, standby；
(2) by Li:Cr: Mn: S molar ratio is standby for weighing a certain amount of lithium nitrate, chromic nitrate, manganese acetate, Manganese monosulfide. by 1.2:0.1: 1.9: 0.03；
(3) weigh citric acid in proportion and hexanediol is configured to mixed solution；
(4) lithium nitrate weighed in step (2), aluminum nitrate and manganese acetate are dissolved in deionized water respectively, add after mix homogeneously in the mixed solution of step (3)；This mixed solution is heated under continuous strong stirring, and Manganese monosulfide. powder load weighted in step (2) is diffused slowly in this mixed solution, being incubated a period of time when temperature is increased to 80 DEG C, until mixed liquor becomes gel, further heat drying becomes xerogel；
(5) xerogel is transferred to 400 DEG C of heat treatments of constant temperature 3 hours in Muffle furnace, it is cooled to room temperature with furnace temperature, 750 DEG C of heat treatments of constant temperature 10 hours in Muffle furnace are placed into after grinding tabletting, it is cooled to 600 DEG C of heat treatments subsequently 8 hours, pulverizes after naturally cooling to room temperature and namely obtain described manganate cathode material for lithium.
Claims (6)
1. a manganate cathode material for lithium, it is characterised in that the formula of described manganate cathode material for lithium is Li1.2MxMn2-xO4-ySy, wherein 0 > x >=0.2,0 > y >=0.2.
2. manganate cathode material for lithium according to claim 1, it is characterised in that described doped chemical M is one or more in Li, Na, K, Mg, Ca, Sr, Ba, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Ag, Ce, Sm, Eu, Al, Si, In, Ga, Ge, Sn, Pb, B, Sb, Bi, Se, Te.
3. the method for manganate cathode material for lithium described in preparation claim 1, it is characterised in that it comprises the steps:
(1) adopting kipp gas generator principle by dilute sulfuric acid and Iron sulfuret. hybrid reaction generation hydrogen sulfide gas, passed into by the gas of generation and generate Manganese monosulfide. precipitation in manganese salt solution, then filtration, washing, drying obtain Manganese monosulfide. pressed powder；
(2) a kind of polynary organic monoacid is proportionally added in a kind of polyhydric alcohol and forms mixed solution；
(3) by lithium salts, manganese salt and additive are dissolved in above-mentioned mixed solution according to a certain percentage, polynary organic monoacid forms chelate with lithium ion and manganese ion etc., whole system is uniform solution, now Manganese monosulfide. pressed powder is scattered in solution, and stir, after ultrasonic disperse, heated solution at 60 90 DEG C of temperature, this chelate and polyhydric alcohol generation esterification, solution becomes colloidal sol, continue to add thermosol and remove unnecessary alcohol to obtain gel, add further and be thermally generated xerogel, by xerogel in Muffle furnace at 400 DEG C isothermal holding 3 10 hours, grind tabletting after being cooled to room temperature and obtain presoma；
(4) it is placed in stove at 750 DEG C of temperature by the presoma obtained in step (3) heat treatment 3-15 hour, is cooled to 600 DEG C subsequently and is incubated 3-10 hour, be subsequently cooled to room temperature, pulverize and obtain described manganate cathode material for lithium.
4. the preparation method of manganate cathode material for lithium according to claim 3, it is characterised in that: described manganese salt be manganese sulfate, manganese chloride, manganese nitrate, manganese acetate one or more.
5. the preparation method of manganate cathode material for lithium according to claim 3, it is characterised in that: described polynary organic monoacid be citric acid, oxalic acid, tartaric acid, benzoic acid, salicylic one or more.
6. the preparation method of manganate cathode material for lithium according to claim 3, it is characterized in that: described polyhydric alcohol be ethylene glycol, 1,2 one propylene glycol, Isosorbide-5-Nitrae fourth two. alcohol, hexanediol, neopentyl glycol, Diethylene Glycol, dipropylene glycol, trimethylolpropane, glycerol one or more.
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| CN113140727A (en) * | 2020-01-17 | 2021-07-20 | 中国科学院物理研究所 | Lithium-activated copper-iron-manganese-based layered oxide material, preparation method and application |
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