CN105185981B - A kind of LiNixMn2-xO4The preparation method of positive electrode - Google Patents

A kind of LiNixMn2-xO4The preparation method of positive electrode Download PDF

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CN105185981B
CN105185981B CN201510506385.3A CN201510506385A CN105185981B CN 105185981 B CN105185981 B CN 105185981B CN 201510506385 A CN201510506385 A CN 201510506385A CN 105185981 B CN105185981 B CN 105185981B
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lini
positive electrode
lithium
nickel
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CN105185981A (en
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方海升
冯福山
杨斌
马文会
姚耀春
杨桂玲
戴永年
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Kunming University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The present invention relates to a kind of LiNixMn2‑xO4The preparation method of positive electrode, belongs to anode material for lithium-ion batteries technical field.Lithium source, nickel source, manganese source and adjuvant are subjected to 0.5 ~ 10h of ball milling mixing first, then 60 ~ 160oPresoma is prepared in drying under the conditions of C, and wherein at least one kind is chloride in lithium source, nickel source, manganese source and adjuvant；The presoma that will be obtained, presses 1 ~ 20 under air or oxygen atmosphereoC/min speed is warming up to 500 ~ 800oC 5 ~ 48h of heated at constant temperature, are subsequently cooled to room temperature, and product after cooling is LiNixMn2‑xO4LiNi is obtained after positive electrode, or washed, dryingxMn2‑xO4Positive electrode.This method proposes raw material chloridising, by introducing chlorion, promotes LiNi during solid phase reactionxMn2‑xO4（0.4≤x≤0.5）Material is grown up and exposes { 111 } crystal face under middle low temperature, so as to it is simple, effectively realize high-performance LiNixMn2‑xO4（0.4≤x≤0.5）The preparation of material.

Description

A kind of LiNixMn2-xO4The preparation method of positive electrode
Technical field
The present invention relates to a kind of LiNixMn2-xO4The preparation method of positive electrode, belongs to anode material for lithium-ion batteries technology Field.
Background technology
Lithium ion battery is due to voltage is high, specific capacity is big, have extended cycle life, self discharge is small, memory-less effect, environment The one kind for the problems such as polluting the advantages that small and receive the extensive concern of people, becoming alleviating energy crisis and environmental pollution is effectively Approach.With application of the lithium ion battery in fields such as electric tool, electric automobiles, higher is proposed to the energy density of battery Requirement, and the energy density of lithium ion battery is heavily dependent on positive electrode, improve positive electrode specific capacity or Voltage is one of main path for obtaining lithium ion battery with high energy density.
Spinel-type nickel lithium manganate cathode material LiNixMn2-xO4（0.4 ≤ x ≤ 0.5）, there are 4.7 V（vs. Li+/Li）Voltage platform, 147 mAh/g of specific capacity or so, than energy up to 690 Wh/kg, higher than LiCoO2、LiMn2O4、 LiFePO4It is a kind of high-energy-density power battery anode material with good application prospect Deng the ratio energy of positive electrode.
Influence LiNixMn2-xO4（0.4≤x≤0.5）The principal element of material property has crystal structure, particle size and crystalline substance Particle shape looks.Recent studies indicate that crystal morphology is the influence factor more more crucial than crystal structure and particle size.Work as system Standby LiNixMn2-xO4（0.4≤x≤0.5）Crystal grain is octahedral shape, when crystal grain exposed surface is { 111 } face, even if institute It is large-sized micro-scale crystal grain to obtain material, and the crystal structure of tube material is not that unordered Fd3m structures are still orderly P4332 structures, all with good chemical property.Although reduce LiNixMn2-xO4（0.4≤x≤0.5）The particle ruler of material The very little high rate performance that can further improve material, but the oxygenolysis in high potential of electrolyte can be aggravated at the same time, so as to dislike Change the cycle performance of material.Therefore, for material itself, preparing bulky grain size has { 111 } exposed crystal face LiNixMn2-xO4（0.4≤x≤0.5）Material is the effective ways for obtaining good comprehensive electrochemical.Obviously, the particle of material Size and pattern are by preparation method and conditional decision.Synthesize LiNixMn2-xO4（0.4≤x≤0.5）The method of material has very much, Including solid phase method, sol-gel process, coprecipitation, molten-salt growth method etc., but the really still solid phase method with practical value, and Solid phase method will control the particle size of material and pattern to be not easy to, the mainly regulation and control sintering temperature reported at present.By carrying High sintering temperature, can promote grain growth and shaping.LiNi is prepared for solid phase methodxMn2-xO4（0.4≤x≤0.5）Material, General sintering temperature will be 800oMore than C, particle just can significantly grow up and expose { 111 } crystal face.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of LiNixMn2-xO4The system of positive electrode Preparation Method.This method proposes raw material chloridising, by introducing chlorion, promotes LiNi during solid phase reactionxMn2-xO4（0.4≤ x ≤0.5）Material is grown up and exposes { 111 } crystal face under middle low temperature, so as to it is simple, effectively realize high-performance LiNixMn2-xO4（0.4 ≤ x ≤ 0.5）The preparation of material, the present invention are achieved through the following technical solutions.
A kind of LiNixMn2-xO4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to 0.5 ~ 10h of ball milling mixing first, then 60 ~ 160oC conditions Presoma is prepared in lower drying, and the wherein molar ratio of lithium source, nickel source and manganese source is 1.0 ~ 1.05：x：2-x（0.4≤ x ≤ 0.5）, and at least one kind is chloride in lithium source, nickel source, manganese source and adjuvant；
（2）By step（1）Obtained presoma, presses 1 ~ 20 under air or oxygen atmosphereoC/min speed is warming up to 500 ~800oC 5 ~ 48h of heated at constant temperature, are subsequently cooled to room temperature, and product after cooling is LiNixMn2-xO4Positive electrode, or through washing Wash, obtain LiNi after dryingxMn2-xO4Positive electrode.
The step（1）In lithium source be lithium carbonate, lithium hydroxide or lithium chloride.
The step（1）In nickel source be nickel oxide, nickel hydroxide, nickel chloride or nickel oxalate.
The step（1）In manganese source be manganese dioxide, manganese carbonate, manganese chloride or manganese oxalate.
The step（1）Middle adjuvant is one kind in oxalic acid, sodium oxalate, ammonium oxalate, ammonium chloride, sodium chloride, potassium chloride Or the mixture of two kinds of arbitrary proportions, the addition of adjuvant is product LiNixMn2-xO4（0.4≤ x ≤0.5）Molal quantity 0.1 ~ 3 times.
Raw material chloridising proposed by the present invention, can mainly be promoted using chlorion during solid phase reaction LiNixMn2-xO4（0.4≤x≤0.5）Granular grows and the effect of shaping so that we be able to can be made under middle low temperature Micron order has the LiNi of { 111 } exposed crystal facexMn2-xO4（0.4≤x≤0.5）Material.
The beneficial effects of the invention are as follows：For raw material after superchlorination, micron order can be made under middle low temperature has { 111 } The LiNi of exposed crystal facexMn2-xO4（0.4≤ x ≤0.5）Material.Due to the LiNi of preparationxMn2-xO4Material granule is micron Level, it is smaller than surface, greatly reduce with side reaction of the electrolyte in high voltage, therefore there is good cycle performance；It is brilliant at the same time Octahedral shape is presented in grain, has { 111 } exposed crystal face that lithium ion is easy to diffusion, therefore have good high rate performance；In addition Micron order, which can be made, by solid phase reaction under middle low temperature using method proposed by the present invention in what is more important has { 111 } the high-performance LiNi of exposed crystal facexMn2-xO4（0.4≤ x ≤0.5）Material, energy consumption substantially reduce, and building-up process It is easily achieved.
Brief description of the drawings
Fig. 1 is without chloride in contrast test raw material（Acetate is lithium source, manganese source and nickel source, other conditions and embodiment 1 Together）The LiNi of Shi Hecheng0.5Mn1.5O4SEM figure；
Fig. 2 is the LiNi that the embodiment of the present invention 1 is prepared0.5Mn1.5O4SEM figure；
Fig. 3 is the LiNi that the embodiment of the present invention 1 is prepared0.5Mn1.5O4XRD diagram；
Fig. 4 is to be prepared in contrast test raw material without chloride（a）It is prepared with embodiment 1（b） LiNi0.5Mn1.5O4Cycle performance figure；
Fig. 5 is to be prepared in contrast test raw material without chloride（a）It is prepared with embodiment 1（b） LiNi0.5Mn1.5O4High rate performance figure.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The LiNi0.5Mn1.5O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 1h first, then 100oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.5：1.5, and lithium source, nickel source, manganese source and auxiliary At least one kind is chloride in agent；Wherein lithium source is LiClH2O, 0.1mol；Nickel source is NiCl2·6H2O, 0.05 mol； Manganese source is MnCl2·4H2O, 0.15mol；Adjuvant is oxalic acid, 0.3 mol；
（2）By step（1）Obtained presoma, in air atmosphere by 20oC/min speed is warming up to 500oC heated at constant temperature 10h, is subsequently cooled to room temperature, and product after cooling is LiNi0.5Mn1.5O4Positive electrode.
Contrast test（Raw material is without chlorination）
The LiNi0.5Mn1.5O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 1h first, then 100oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.5：1.5, and lithium source, nickel source, manganese source and auxiliary There is no chloride in agent；Wherein lithium source is lithium acetate, 0.1mol；Nickel source is nickel acetate, 0.05 mol；Manganese source is manganese acetate, 0.15mol；Adjuvant is oxalic acid, 0.3 mol；
（2）By step（1）Obtained presoma, in air atmosphere by 20oC/min speed is warming up to 500oC constant temperature adds Hot 10h, is subsequently cooled to room temperature, and product after cooling is LiNixMn2-xO4Positive electrode.
The LiNi that contrast test is preparedxMn2-xO4Positive electrode SEM is schemed as shown in Figure 1, what embodiment 1 was prepared LiNi0.5Mn1.5O4Positive electrode is as shown in Fig. 2, the LiNi that embodiment 1 is prepared0.5Mn1.5O4XRD diagram as shown in figure 3, reality Apply the LiNi that example 1 is prepared0.5Mn1.5O4（b）The LiNi being prepared with contrast test0.5Mn1.5O4（a）Chemical property As shown in Figure 4 and Figure 5.Fig. 2 compared to Figure 1, after raw material chlorination, substantially grow up by particle, and presentation has { 111 } exposed crystal face Octahedral shape.Fig. 3 is that the XRD of 1 products therefrom of embodiment is composed, and is pure LiNi0.5Mn1.5O4, wherein Si is artificially to add Internal standard.It was found from Fig. 4 and Fig. 5 contrasts, synthesis gained bulky grain LiNi after raw material chlorination0.5Mn1.5O4, due to { 111 } The octahedral shape of exposed crystal face, beneficial to the quick diffusion of lithium ion, therefore has more preferable chemical property.
Embodiment 2
The LiNi0.5Mn1.5O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 3h first, then 100oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.5：1.5, and lithium source, nickel source, manganese source and auxiliary At least one kind is chloride in agent；Wherein lithium source is LiOHH2O, 0.1mol；Nickel source is NiO, 0.05 mol；Manganese source is MnCl2·4H2O, 0.15mol；Adjuvant is oxalic acid, 0.25 mol；
（2）By step（1）Obtained presoma, in air atmosphere by 10oC/min speed is warming up to 600oC constant temperature adds Hot 10h, is subsequently cooled to room temperature, and product after cooling is LiNi0.5Mn1.5O4Positive electrode.
Embodiment 3
The LiNi0.5Mn1.5O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 3h first, then 80oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.5：1.5, and lithium source, nickel source, manganese source and auxiliary At least one kind is chloride in agent；Wherein lithium source is Li2CO3, 0.05mol；Nickel source is NiO, 0.05mol；Manganese source is MnCl2·4H2O, 0.15mol；Adjuvant is ammonium oxalate, 0.15 mol；
（2）By step（1）Obtained presoma, in air atmosphere by 20oC/min speed is warming up to 700oC constant temperature adds Hot 10h, is subsequently cooled to room temperature, and product after cooling is LiNi0.5Mn1.5O4Positive electrode.
Embodiment 4
The LiNi0.5Mn1.5O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 6h first, then 80oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.5：1.5, and lithium source, nickel source, manganese source and auxiliary At least one kind is chloride in agent；Wherein lithium source is Li2CO3, 0.05mol；Nickel source is Ni (OH)2, 0.05mol；Manganese source is MnCO3·4H2O, 0.15mol；Adjuvant is ammonium chloride, 0.1 mol；
（2）By step（1）Obtained presoma, presses 5 under oxygen atmosphereoC/min speed is warming up to 700oC heated at constant temperature 20h, is subsequently cooled to room temperature, and product after cooling is LiNi0.5Mn1.5O4Positive electrode.
Embodiment 5
The LiNi0.45Mn1.55O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 3h first, then 100oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.02：0.45：1.55, and lithium source, nickel source, manganese source with it is auxiliary At least one kind is chloride in auxiliary agent；Wherein lithium source is Li2CO3, 0.051mol；Nickel source is NiO, 0.045mol；Manganese source is MnCl2·4H2O, 0.155mol；Adjuvant is sodium oxalate, 0.155mol；
（2）By step（1）Obtained presoma, in air atmosphere by 20oC/min speed is warming up to 800oC heated at constant temperature 15h, is subsequently cooled to room temperature, and products therefrom is washed, obtains LiNi after drying0.45Mn1.55O4Positive electrode.
Embodiment 6
The LiNi0.4Mn1.6O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 6h first, then 120oDry system under the conditions of C Standby to obtain presoma, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.4：1.6, and lithium source, nickel source, manganese source and auxiliary At least one kind is chloride in agent；Wherein lithium source is Li2CO3, 0.05mol；Nickel source is NiC2O4·2H2O, 0.04mol；Manganese source For MnC2O4·4H2O, 0.16mol；Adjuvant is potassium chloride（0.05mol）And sodium chloride（0.05mol）；
（2）By step（1）Obtained presoma, presses 10 under oxygen atmosphereoC/min speed is warming up to 700oC heated at constant temperature 10h, is subsequently cooled to room temperature, and product after cooling is washed, obtains LiNi after drying0.4Mn1.6O4Positive electrode.
Embodiment 7
The LiNi0.4Mn1.6O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 0.5h first, then 60oIt is dry under the conditions of C Presoma is prepared, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.4：1.6, and lithium source, nickel source, manganese source with it is auxiliary At least one kind is chloride in auxiliary agent；Wherein lithium source is Li2CO3, 0.05mol；Nickel source is NiC2O4·2H2O, 0.04mol；Manganese Source is MnC2O4·4H2O, 0.16mol；Adjuvant is sodium chloride, 3mol；
（2）By step（1）Obtained presoma, in air atmosphere by 1oC/min speed is warming up to 800oC heated at constant temperature 5h, is subsequently cooled to room temperature, and product after cooling is washed, obtains LiNi after drying0.4Mn1.6O4Positive electrode.
Embodiment 8
The LiNi0.4Mn1.6O4The preparation method of positive electrode, it is comprised the following steps that：
（1）Lithium source, nickel source, manganese source and adjuvant are subjected to ball milling mixing 10h first, then 160oIt is dry under the conditions of C Presoma is prepared, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0：0.4：1.6, and lithium source, nickel source, manganese source with it is auxiliary At least one kind is chloride in auxiliary agent；Wherein lithium source is Li2CO3, 0.05mol；Nickel source is NiC2O4·2H2O, 0.04mol；Manganese Source is MnC2O4·4H2O, 0.16mol；Adjuvant is sodium chloride, 0.01mol；
（2）By step（1）Obtained presoma, in air atmosphere by 10oC/min speed is warming up to 500oC heated at constant temperature 48h, is subsequently cooled to room temperature, and product after cooling is washed, obtains LiNi after drying0.4Mn1.6O4Positive electrode.
The embodiment of the present invention is explained in detail above in association with attached drawing, but the present invention is not limited to above-mentioned Embodiment, within the knowledge of a person skilled in the art, can also be before present inventive concept not be departed from Put that various changes can be made.

Claims (4)

  1. A kind of 1. LiNixMn2-xO4The preparation method of positive electrode, it is characterised in that comprise the following steps that：
    （1）Lithium source, nickel source, manganese source and adjuvant are subjected to 0.5 ~ 10h of ball milling mixing first, then 60 ~ 160oDone under the conditions of C Dry that presoma is prepared, the wherein molar ratio of lithium source, nickel source and manganese source is 1.0 ~ 1.05：x：2-x, 0.4≤x≤0.5；
    （2）By step（1）Obtained presoma, presses 1 ~ 20 under air or oxygen atmosphereoC/min speed is warming up to 500 ~ 800oC 5 ~ 48h of heated at constant temperature, are subsequently cooled to room temperature, and product after cooling is LiNixMn2-xO4Positive electrode, or through washing Wash, obtain LiNi after dryingxMn2-xO4Positive electrode；
    The step（1）Middle adjuvant is the mixture of one or both of ammonium chloride, sodium chloride, potassium chloride arbitrary proportion, The addition of adjuvant is product LiNixMn2-xO40.1 ~ 3 times of molal quantity.
  2. 2. LiNi according to claim 1xMn2-xO4The preparation method of positive electrode, it is characterised in that：The step（1） In lithium source be lithium carbonate or lithium hydroxide.
  3. 3. LiNi according to claim 1xMn2-xO4The preparation method of positive electrode, it is characterised in that：The step（1） In nickel source be nickel oxide, nickel hydroxide or nickel oxalate.
  4. 4. LiNi according to claim 1xMn2-xO4The preparation method of positive electrode, it is characterised in that：The step（1） In manganese source be manganese dioxide, manganese carbonate or manganese chloride.
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