CN106673075B - A kind of modified O3 type sodium-ion battery layered cathode material and its preparation method and application - Google Patents

A kind of modified O3 type sodium-ion battery layered cathode material and its preparation method and application Download PDF

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CN106673075B
CN106673075B CN201710003808.9A CN201710003808A CN106673075B CN 106673075 B CN106673075 B CN 106673075B CN 201710003808 A CN201710003808 A CN 201710003808A CN 106673075 B CN106673075 B CN 106673075B
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CN106673075A (en
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郭玉国
王鹏飞
殷雅侠
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Institute of Chemistry CAS
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Abstract

The invention discloses a kind of modified O3 type sodium-ion battery layered cathode materials and its preparation method and application.The method of modifying is to introduce metal ion (such as Ti of non-electroactive in situ in transition metal oxide layer, Li, Mg, Zn, Cu, Sn it) is modified, this method preparation is simple, the positive electrode uniform particle diameter being synthesized, Elemental redistribution is uniform, raw material is easy to get, it is cheap, degree of being practical is high, and the storage stability of the structural stability and exposure air in material charge and discharge process can be greatly improved when taking the positive electrode assembling sodium-ion battery of this method modification, therefore the positive electrode of modified shows excellent cyclical stability and high rate performance, this method has a good application prospect in optimization sodium-ion battery energy storage device performance and universality.

Description

A kind of modified O3 type sodium-ion battery layered cathode material and its preparation method and application
Technical field
The invention belongs to field of chemical power source, also belong to technical field of energy material.More particularly to a kind of modified O3 type sodium Ion battery layered cathode material, thus improves O3 type sodium-ion battery layered cathode material at the preparation method of the positive electrode The method of charge and discharge process structural stability and air stability, and existed using novel sodium-ion battery prepared by this method Application in energy storage device.
Background technique
Compared to the lithium resource of shortage, sodium element global range is widely distributed, low raw-material cost, thus is storing up on a large scale Sodium-ion battery has more the potentiality of sustainable development than lithium ion battery in energy device.However the sodium-ion battery currently reported is just Pole material capacity is but far below cathode, therefore promotes positive electrode performance as the key for improving sodium-ion battery energy density.
In recent years, transition metal stratiform structure oxide NaxTMO2(TM is transition metal element) is since specific capacity is high, system The series of advantages such as Preparation Method is simple and environmental-friendly and paid close attention to by researcher.However, this kind of material is in cyclic process In, it is easy to happen irreversible phase transformation, it is very poor in charge and discharge process structural stability so as to cause such material.And this kind of material In air, the moisture in air can be embedded into transition metal interlayer for material storage, so that irreversible change occurs for material structure, also can Battery performance is influenced, also limitation O3 profile material is further practical, in order to solve these problems, in layer structure transiting metal oxidation Layer introduces non-electroactive and can be simultaneously with metal ion similar in initial transition metal ion radius (such as Li, Ti, Sn etc.) Storage stability is when improving structural stability and exposure air of the positive electrode in charge and discharge process so as to improve cell performance Energy.
The present invention selects the O3-NaNi of rhombohedral phase respectively0.5Mn0.5O2For basis material, creatively pass through control reaction Condition introduces metal ions M (such as Li, Ti, Zn, Mg, Cu, the Sn, and to gold of non-electroactive in raw material crystal structure Belong to M content to be regulated and controled, compare different synthetic methods, optimization uses the O3-Na (Ni of Solid phase synthesis0.5Mn0.5)1-xMxO2Sodium from Sub- cell positive material appearance and size is small, and uniform particle diameter, Elemental redistribution is more uniform, and this kind of titanium base material is used as sodium-ion battery When positive, the irreversible transition that charge and discharge process can effectively inhibit material to occur, so that height ratio capacity is shown, height electric discharge electricity Pressure, the excellent feature of battery performance, and since the metal ion of non-electroactive introduces, transition metal interlamellar spacing reduces, The insertion of moisture in air is limited, the storage stability of material is greatly improved, this is in the following extensive energy storage of sodium-ion battery It has broad application prospects in practicalization.
Summary of the invention
The object of the present invention is to provide a kind of modified O3 type sodium-ion battery layered cathode materials and preparation method thereof, and Stable storage when a kind of raising O3 type sodium-ion battery layered cathode material charge and discharge process structural stability and exposure air The method of property.
Present invention firstly provides a kind of raising O3 type sodium-ion battery layered cathode material charge and discharge process structural stabilities Method, which comprises in O3 type positive electrode NaNi0.5Mn0.5O2The transition metal layer of basis material introduces non-in situ Electro-chemical activity and ionic radius and Ni2+, Mn4+Similar metal ion, the metal ion are preferred are as follows: Li, Ti, Mg, Zn Cu, more preferably Li, Ti, Sn.
In addition, the present invention for thinking above, also provides a kind of modified O3 type sodium-ion battery layered cathode material, Described in positive electrode transition metal layer in situ introduce non-electroactive metal ion formed O3 type positive electrode, specifically Composition are as follows: O3-Na (Ni0.5Mn0.5)1-xMxO2, wherein M=Li, Ti, Mg, Zn Cu's one or more, 0 < x < 0.5.It is preferred that M is Li,Ti,Sn。
The particle size of the positive electrode is preferably 1-2 μm, compacted density 4.5-5.0g/cm3, preferably 4.7- 5.0g/cm3。
The present invention further provides the method for preparing anode material, include the following steps: metal oxide in solvent Mid-early stage ball milling mixing is uniform, is heat-treated by the early stage of drying, tabletting, and then temperature programming calcines to obtain the positive electrode.
In above-mentioned preparation method, the material purity is all larger than 99%.
In above-mentioned preparation method, pressure is 10-20MPa. when tabletting
In above-mentioned preparation method, calcination temperature is 800-1000 DEG C, preferably 900 DEG C.
In above-mentioned preparation method, calcination time 15h-24h.Preferably 15h, in the heating step, heating rate is 5-15℃min-1, preferably 5 DEG C of min-1。
Application provided by the present invention is the O3-Na (Ni based on O3 type rhombohedral phase0.5Mn0.5)1-xMxO2Material as sodium from The application of sub- anode of secondary battery.
The present invention also provides a kind of sodium-ion battery combination electrodes and preparation method thereof, which contains the O3- Na(Ni0.5Mn0.5)1-xMxO2Positive electrode, binder and conductive additive.It prepares the combination electrode and specifically includes following step It is rapid: the positive electrode and conductive additive, binder and solvent to be mixed in a certain ratio, through works such as slurrying, smear, dryings Skill process obtains compound anode.
In the above method, the conductive additive be one of carbon black, Super-P, Ketjen black or a variety of, preferably Super-P。
In the above method, the binder and solvent are that Kynoar (PVDF) (is with N-Methyl pyrrolidone (NMP) Solvent) or polyacrylic acid (PAA), sodium carboxymethylcellulose (CMC), sodium alginate (SA), in gelatin (taking water as a solvent) It is one or more, preferably PVDF.
Sodium-ion battery provided by the invention, including as cathode metallic sodium, as anode aforementioned positive electrode compound And organic electrolyte.
In above-mentioned battery, the organic electrolyte is carbonic ester electrolyte, concentration 0.1-2M, preferably 1M.
In the carbonic ester electrolyte, solvent is selected from dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), at least one of ethylene carbonate (EC) and propene carbonate (PC), preferably EC:DEC=1:1；Solute is selected from six Sodium fluoro phosphate (NaPF6), sodium perchlorate (NaClO4), one of two (trimethyl fluoride sulfonyl) imines sodium (NaTFSI) or a variety of, Preferably sodium hexafluoro phosphate (NaPF6)。
25 DEG C of the operating temperature of the sodium-ion battery.
Detailed description of the invention
Fig. 1 is the NaNi of sol-gal process preparation in embodiment 10.5Mn0.4Ti0.1O2The scanning electron microscopic picture of material.
Fig. 2 is the NaNi of the solid phase method preparation in comparative example 10.5Mn0.5O2The scanning electron microscopic picture of material.
Fig. 3 is the NaNi that in embodiment 1 prepared by sol-gal process0.5Mn0.4Ti0.1O2The transmission electron microscope Elemental redistribution of material Figure, it was demonstrated that element ti is evenly distributed in material.
Fig. 4 is the NaNi in embodiment 10.5Mn0.4Ti0.1O2The charging and discharging curve of material.
Fig. 5 is the NaNi in embodiment 10.5Mn0.4Ti0.1O2Long circulating performance curve under material 1C.
Fig. 6 is XRD comparison diagram after material exposure air 10 days in embodiment 1 and comparative example 1.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Experimental method described in following embodiments, unless otherwise specified, the reagent and material commercially obtain ?.
Embodiment 1
(1) NaNi is prepared0.5Mn0.4Ti0.1O2Positive electrode
Accurately weigh corresponding proportion Na2CO3、Mn2O3、NiO、TiO2For 24 hours, 20MPa pressure depresses to diameter 14mm's to ball milling Disk, 950 DEG C of calcining 15h obtain black powder.The size for obtaining powder particle is 5-10 μm, density 5.1g/cm3。
The particle size obtained as can be seen from comparison with Figure 1 and Figure 2 is at 3-5 μm, and uniform particle diameter, pattern is very regular, element Distribution Ti highly uniform on particle.
(2) NaNi is prepared0.5Mn0.5-yTi0.1O2Compound anode
The positive electrode of above-mentioned preparation is mixed with Super P, binder polyvinylidene fluoride 7:2:1 in mass ratio, and Solvent N-methyl pyrilidone is added, obtains compound anode through process flows such as slurrying, smear, dryings.
(3) sodium-ion battery is assembled
The compound anode of above-mentioned preparation is assembled into sodium-ion battery with metallic sodium cathode, electrolyte selects carbonic ester electrolysis Liquid (1M NaPF6EC/DEC (volume ratio 1:1) solution).
(4) sodium-ion battery is tested
Using charge and discharge instrument, to above-mentioned sodium-ion battery, the 0.1C in carbonic ester electrolyte (is equivalent to 24mA g-1) under multiplying power Carry out constant current charge-discharge test.Fig. 4 is that sodium-ion battery 0.1C in carbonic ester electrolyte (is equivalent to 24mA g-1) multiplying power Under charging and discharging curve.The NaNi from attached drawing 40.5Mn0.4Ti0.1O2The sodium-ion battery charge and discharge that material is assembled as positive electrode Electric curve can be seen that battery 3.0V average discharge volt with higher, and reversible discharge specific capacity is in 131mA h/g.From In attached drawing 5, uses cycle performance curve of the material in the sodium-ion battery as anode assembling to can be seen that battery and show Excellent cyclical stability, in 1C multiplying power (240mA g-1) circulation 200 after circle, stablize in 107.5mA h/g, holds by specific discharge capacity Conservation rate is measured 84% or more.And the material, after exposure air 10 days, crystal structure remains intact, and illustrates in transition gold Category oxide layer, which introduces non-electroactive ion Ti, can effectively improve the structural stability and air-stable of material circulation process Property.
Embodiment 2
Prepare NaNi0.5Mn0.3Ti0.2O2, in addition to reactant feed ratio is different, remaining is same as Example 1.Obtain powder The size of last particle is 3-7 μm, density 5.0g/cm3。
Embodiment 3
Prepare NaNi0.5Mn0.2Ti0.3O2, in addition to reactant feed ratio is different, remaining is same as Example 1.Obtain powder The size of last particle is 5-8 μm, density 5.0g/cm3。
Embodiment 4
Prepare NaNi0.5Mn0.1Ti0.4O2, in addition to reactant feed ratio is different, remaining is same as Example 1.Obtain powder The size of last particle is 5-10 μm, density 5.1g/cm3。
Embodiment 5
Prepare NaNi0.5Mn0.4Li0.1O2, in addition to reactant TiO2Replace with Li2CO3, feed ratio is different, remaining with reality It is identical to apply example 1.The size for obtaining powder particle is 3-5 μm, density 4.9g/cm3。
Embodiment 6
Prepare NaNi0.5Mn0.4Sn0.1O2, in addition to reactant TiO2Replace with SnO2, feed ratio is different, remaining with implementation Example 1 is identical.The size for obtaining powder particle is 3-5 μm, density 4.9g/cm3。
Comparative example 1
(1) solid phase method prepares NaNi0.5Mn0.5O2Positive electrode
Accurately weigh corresponding proportion Na2CO3、Mn2O3、NiO2For 24 hours, 20MPa pressure depresses to the disk of diameter 14mm to ball milling, 1000 DEG C of calcining 15h obtain black powder.The size for obtaining powder particle is 5-10 μm, density 5.1g/cm3。
(2) NaNi is prepared0.5Mn0.5O2Compound anode (the specific steps are the same as those in embodiment 1)
(3) assemble sodium-ion battery (the specific steps are the same as those in embodiment 1)
(4) sodium-ion battery test (the specific steps are the same as those in embodiment 1)
Comparative example 2
Prepare NaNi0.4Mg0.1Mn0.5O2, in addition to reactant increases MgO, feed ratio is different, remaining with 1 phase of comparative example Together.The size for obtaining powder particle is 1-2 μm, density 4.7g/cm3。
Comparative example 3
Prepare NaNi0.4Zn0.1Mn0.5O2, in addition to reactant increases ZnO, feed ratio is different, remaining with 1 phase of comparative example Together.The size for obtaining powder particle is 3-5 μm, density 4.8g/cm3。
Comparative example 4
Prepare NaNi0.4Cu0.1Mn0.5O2, in addition to reactant increases CuO, feed ratio is different, remaining with 1 phase of comparative example Together.The size for obtaining powder particle is 2-5 μm, density 5.0g/cm3。
The experimental data of 1 embodiment and comparative example of table
From subordinate list battery performance and air stability comparison as can be seen that O3-Na (Ni0.5Mn0.5)1-xMxO2(M=Li, Ti, Sn) specific discharge capacity and capacity retention ratio, the material property than being not added in any modification comparative example 1 is good, shows that material fills Discharging structure stability is largely increased, and passes through the O3-Na (Ni of comparison different proportion Ti modification0.5Mn0.5)1-xTixO2Material Performance finds the material cell best performance of 0.1≤x≤0.3, and in comparative example 1-4 after material exposure air 10 days, structure It has been destroyed, and has passed through Li, the crystal structure of the material of Ti, Sn modification can also be kept well, hence it is demonstrated that in mistake Cross metal oxide layer introduce non-electroactive ion (preferably Li, Ti, Sn) can effectively improve material circulation process structure it is steady Qualitative and air stability.
In conclusion provided by the invention in O3 type NaNi0.5Mn0.5O2The transition metal layer of basis material introduces non-in situ Metal ion Li, Ti, the Sn simple possible of electro-chemical activity, cyclical stability and air stability greatly improve, compared to first Beginning O3-NaNi0.5Mn0.5O2The structural stability of basis material, material charge and discharge process is largely increased, the sodium ion of assembling Battery can have higher average discharge volt simultaneously by reversible specific capacity with higher at room temperature, and room temperature cycles are steady It is qualitative excellent, mainly form O3-Na (Ni0.5Mn0.5)1-xMxO2Method for preparing anode material is simple, and raw material is easy to get, and price is low Honest and clean thus of the invention sodium-ion battery is expected to as a kind of novel high-energy density energy storage device, and has good answer Use prospect.
Above content is merely a preferred embodiment of the present invention, and is not intended to limit embodiment of the present invention, and this field is general Logical technical staff's central scope according to the present invention and spirit can very easily carry out corresponding flexible or modification, therefore Protection scope of the present invention should be subject to protection scope required by claims.

Claims (1)

1. a kind of O3 type sodium-ion battery layered cathode material charge and discharge process structural stability and air stability of improving Method, which comprises in O3 type positive electrode NaNi0.5Mn0.5O2The transition metal layer of basis material introduces non-electrical in situ Chemical activity and ionic radius and Ni2+, Mn4+Similar Sn metal ion is being formed by modified O3 type sodium-ion battery stratiform just Pole material, concrete composition are as follows: O3-NaNi0.5Mn0.4Sn0.1O2, particle size is 3-5 μm, the pressure of the positive electrode particle Real density is 4.9g/cm3。
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