CN104495959A - Positive electrode material of sodium ion secondary battery, preparation method of positive electrode material, as well as lithium-sodium mixed battery - Google Patents

Positive electrode material of sodium ion secondary battery, preparation method of positive electrode material, as well as lithium-sodium mixed battery Download PDF

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Publication number
CN104495959A
CN104495959A CN201410765652.4A CN201410765652A CN104495959A CN 104495959 A CN104495959 A CN 104495959A CN 201410765652 A CN201410765652 A CN 201410765652A CN 104495959 A CN104495959 A CN 104495959A
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positive electrode
electrode material
ion secondary
secondary battery
lithium
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杜菲
姚晔
魏英进
王春忠
陈岗
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Jilin University
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Jilin University
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    • 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 invention provides a positive electrode material of a sodium ion secondary battery and belongs to the field of lithium-sodium mixed batteries. The molecular formula of the material is Li2RuO3. The invention further provides a preparation method of the positive electrode material of the sodium ion secondary battery. The method comprises the following steps: mixing oxide containing lithium with oxide containing ruthenium, and carrying out wet grinding to obtain mixture powder; then pressing the obtained mixture powder into sheets; and sintering to obtain the positive electrode material of the sodium ion secondary battery. The invention further provides the lithium-sodium mixed battery prepared from the positive electrode material. The lithium-sodium mixed battery has the relatively high specific capacity and the relatively good circulating performance; and an experiment result shows that constant-current charging/discharging is carried out at a voltage interval being 2.0V-4.0V at a current density being 100mAh/g, the discharging specific capacity is up to 150mAg/g, and the charging/discharging specific capacity is stabilized to be about 140mAg/g after 50 times of cycles.

Description

A kind of sodium ion secondary battery positive electrode material, preparation method and lithium sodium hybrid battery
Technical field
The invention belongs to lithium sodium hybrid battery field, be specifically related to a kind of sodium ion secondary battery positive electrode material, preparation method and lithium sodium hybrid battery.
Background technology
Along with industrial expansion, energy problem becomes the focus that people pay close attention to.The current world utilize 85% of the energy to come from fossil feedstock (coal, oil, Sweet natural gas etc.), these raw materials are non-renewable, and its environmental pollution caused is also in continuous aggravation.Therefore, the development of green energy resource and material thereof, for realizing the 21st century strategy of sustainable development, alleviating energy crisis and alleviate environmental pollution pressure and all have very important significance.Lithium ion battery, as a kind of efficient green new forms of energy that can be recycled, is a kind of important technology approach comprehensively alleviating the energy, resources and environment problem.Along with the continuous lifting of various portable type electronic product performance, the arrival of 4G communication times, the fast development of the emerging technologies such as electromobile and extensive energy storage, proposes more and more higher requirement to indexs such as lithium ion battery energy density, power density, life-span and securities.
Since first piece of commercial Li-ion batteries in 1991 is come out, world's lithium ion battery industry obtains develop rapidly.Current most of lithium ion battery still uses LiCoO 2make positive electrode material, but on the earth, the reserves of cobalt resource are very limited (only accounting for 20/1000000ths of earth crustal mass).In addition, adopt the lithium ion battery of this material in use also to there is the potential safety hazards such as larger on fire, blast, be unsuitable for requiring strict power-type lithium ion battery to safety performance.As everyone knows, sodium reserved resources is on earth enriched, and compare with lithium and have great advantage, in recent years, sodium-ion battery caused people and more and more pays close attention to.But the capacity due to sodium-ion battery can not reach the level of lithium ion battery, therefore, finding safety, efficiently Novel lithium sodium hybrid battery positive electrode material is the target of scientific circles and an industry member long-sought.
Emerged a collection of material with excellent electrochemical performance in recent years, as: lithium manganate (LiMn 2o 4), iron lithium phosphate (LiFePO 4), ternary layered material (LiCo 1-2xni xmn xo 2), rich lithium lamellar compound xLi 2mnO 3_ (1-x) LiMnO 2and fluorosulfuric acid salt LiFeSO 4f etc.In numerous positive electrode material, there is the material of stratiform attribute with its stable structure, the transmission path of maximum dimension can be provided to become the main force of anode material of lithium battery research for lithium ion.
The molecular formula formed with 3d transition metal ion is for LiMO 2positive electrode material, as LiCoO 2and LiNiO 2studied widely, present people are conceived to again 4d/5d transition metal and are formed Li with+4 valencys 2qO 3positive electrode material because the transition of electronics is mainly via M in 3d positive electrode material 3+-O 2--M 3+superexchange or bialternative series realize, between strong electronics, exchange interaction (Coulomb repulsion energy U) will increase band gap width, reduce the electronic conductivity of material, so 3d layered cathode material is generally Mott-Hubbard isolator.And the outer shell electronic configuration forming stratified material by 4d/5d transition metal mostly is low spin state, as: Mo 4+(4d 2, t 2g 2), Ru 4+(4d 3, t 2g 3) and Ir 4+(5d 5, t 2g 5).Compared with e gelectronic orbit, t 2gcorrelation electron system has larger track degree of freedom and ductility, therefore in transition metal layer along t 2gorbital direction (xy, yz or zx) on more easily form the overlapping of electronic cloud, directly do not form Q by the exchange interaction of O ion 4+-Q 4+metallic bond, the therefore good conductor of 4d/5d transition metal stratiform material normally electronics.Li in 4d transition metal positive electrode material 2ruO 3the extensive concern of investigator is being obtained in recent years with the high theoretical capacity of 328mAh/g.
A lot of seminar is to Li 2ruO 3had relevant research and report, although make some progress for the research of ruthenium base stratified material, still there is many problem in science is worth further inquiring into.The charging and discharging capacity of general sodium-ion battery positive material is approximately 80-120mAh/g, does not have bibliographical information at present by Li 2ruO 3for sodium-ion battery positive material.
Summary of the invention
The object of the invention is to solve the low problem of existing sodium-ion battery positive material charging and discharging capacity, and a kind of sodium ion secondary battery positive electrode material, preparation method and lithium sodium hybrid battery are provided.
First the present invention provides a kind of sodium ion secondary battery positive electrode material, and the molecular formula of this material is Li 2ruO 3, spacer C2/c.Unit cell parameters: α=90, β=108.5, γ=90.
The present invention also provides a kind of preparation method of sodium ion secondary battery positive electrode material, comprising:
Step one: by containing the carbonate of lithium and mixing containing the oxide compound of ruthenium, carry out wet-milling, obtain mix powder;
Step 2: mix powder tabletted step one obtained, sinters, and obtains sodium ion secondary battery positive electrode material.
Preferably, the described carbonate containing lithium is Li 2cO 3.
Preferably, the described oxide compound containing ruthenium is RuO 2.
Preferably, the described wet-milling time is 1-2 hour.
Preferably, in the described carbonate containing lithium and the oxide compound containing ruthenium, the mol ratio of Li and Ru is 2:1.
Preferably, the sintering temperature of described step 2 is 900-1000 DEG C, and sintering time is 20-24 hour.
The lithium sodium hybrid battery that the present invention also provides above-mentioned sodium ion secondary battery positive electrode material to prepare.
Beneficial effect of the present invention
First the present invention provides a kind of sodium ion secondary battery positive electrode material, and the molecular formula of this material is Li 2ruO 3, the present invention is first by Li 2ruO 3use as sodium ion secondary battery positive electrode material.
The present invention also provides a kind of preparation method of sodium ion secondary battery positive electrode material, and the method mixes by the oxide compound containing lithium with containing the oxide compound of ruthenium, carries out wet-milling, obtain mix powder; Then the mix powder tabletted will obtained, sinters, and obtains sodium ion secondary battery positive electrode material.Compare with prior art, preparation method of the present invention is simple, cost is lower, is applicable to large-scale commercial production.
The lithium sodium hybrid battery that the present invention also provides a kind of above-mentioned sodium ion secondary battery positive electrode material to prepare, this lithium sodium hybrid battery has higher specific storage and has good cyclical stability, experimental result shows: carry out constant current charge-discharge at 2.0-4.0V voltage range with the current density of 100mAh/g, specific discharge capacity is up to 150mAh/g, after 50 circulations, charging and discharging capacity is stabilized in about 140mAh/g.
Accompanying drawing explanation
The powdered material Li of Fig. 1 prepared by the embodiment of the present invention 1 2ruO 3x-ray diffraction (XRD) collection of illustrative plates.
The powdered material Li of Fig. 2 prepared by the embodiment of the present invention 1 2ruO 3electronic Speculum (SEM) collection of illustrative plates.
The powdered material Li of Fig. 3 prepared by the embodiment of the present invention 1 2ruO 3the charging and discharging curve figure (current density is 100mAh/g, voltage range 2.0-4.0V) of the 1st, 2,3 week in Na ionization cell.
The powdered material Li of Fig. 4 prepared by the embodiment of the present invention 1 2ruO 3cycle performance figure (current density is 100mAh/g, voltage range 2.0-4.0V).
Embodiment
First the present invention provides a kind of sodium ion secondary battery positive electrode material, and the molecular formula of this material is Li 2ruO 3, spacer C2/c, unit cell parameters: α=90, β=108.5, γ=90.This material is made up of lithium layer and transition metal layer, and transition metal layer is then by 1/3Li +ion and 2/3Q 4+ion occupies jointly, and forms the superlattice ordered state of " honeycomb (the honeycomb) " type of [LiQ6].
The present invention also provides a kind of preparation method of sodium ion secondary battery positive electrode material, comprising:
Step one: by containing the carbonate of lithium and mixing containing the oxide compound of ruthenium, carry out wet-milling, obtain mix powder;
Step 2: mix powder tabletted step one obtained, sinters, and obtains sodium ion secondary battery positive electrode material.
According to the present invention, described in step one by containing lithium carbonate and mix containing the oxide compound of ruthenium, carry out wet-milling, obtain mix powder; The described described carbonate containing lithium is preferably Li 2cO 3, the described oxide compound containing ruthenium is preferably RuO 2, in the described carbonate containing lithium and the oxide compound containing ruthenium, the mol ratio of Li and Ru is preferably 2:1.Described wet-milling, be grind being dissolved in solvent after the carbonate containing lithium and the mixing of the oxide compound containing ruthenium, described solvent preferred alcohol or acetone, the wet-milling time is preferably 1-2 hour.Wet-milling can make raw material mixture homogeneity better, and can shorten mixing time.
According to the present invention, mix powder obtained above is preferably pressed into the thin slice of 2 ~ 3mm at the pressure of 18 ~ 22MPa, is placed in corundum crucible, sinters in retort furnace, last naturally cooling, grind into powder, obtain sodium ion secondary battery positive electrode material.Described sintering temperature is preferably 900-1000 DEG C, and temperature rise rate is preferably 5 DEG C/min, and sintering time is preferably 20-24 hour.
The lithium sodium hybrid battery that the present invention also provides above-mentioned sodium ion secondary battery positive electrode material to prepare.The preparation method of lithium sodium hybrid battery of the present invention is the technological method that this area is commonly used, and is not particularly limited, preferably includes: by the Li prepared 2ruO 3material, conductive auxiliary agent and binding agent are mixed into slurry according to certain mass ratio, and concrete ratio can regulate as requested, is not particularly limited, the preferred Li of the present invention 2ruO 3material, acetylene black and PVDF (polyvinylidene difluoride (PVDF)) are mixed into slurry according to the ratio of mass ratio 8:1:1, afterwards by obtained slurry even application in aluminum substrates, by the electrode slice drying more than 10 hours in vacuum drying oven obtained, pressing treatment is carried out to the electrode slice of drying, then the pole piece of system is cut into size be applicable to thin slice as positive pole, in the glove box being full of argon gas (content of water and oxygen is less than 1PPM) be assembled into experimental cell.The present invention is half-cell to electrode with pure sodium sheet, and the barrier film of battery adopts GLASSMICROFIBER FILTERS GF/C tMbarrier film, electrolytic solution can adopt various types of liquid electrolyte or solid electrolyte, and the present invention is preferably to be dissolved in the organic electrolyte of PC solvent containing 1mol/L sodium perchlorate.Experimental cell carries out charge and discharge cycles test by by computer-controlled auto charge and discharge instrument.
Below in conjunction with specific embodiment, further detailed description is done to the present invention.The raw material related in embodiment is all from Sigma-Aldrich.
Embodiment 1
Take 1mol Li 2cO 3with 1mol RuO 2put into agate mortar, add dehydrated alcohol and carry out wet-milling 1 hour, obtain mix powder; Mix powder is carried out compressing tablet, the thin slice of 2 ~ 3mm is pressed into the pressure of 18MPa, be placed in corundum crucible, sinter at the temperature of 950 DEG C in retort furnace, temperature rise rate is 5 DEG C/min, sintering time 22 hours, last naturally cooling, grind into powder afterwards, obtains sodium ion secondary battery positive electrode material Li 2ruO 3.
Fig. 1 is Li prepared by the embodiment of the present invention 1 2ruO 3x-ray diffraction (XRD) collection of illustrative plates of powdered material.Specific experiment method is: use the Bruker D8 diffractometer being equipped with copper target X-ray tube to carry out X-ray powder diffraction test to sample.Sample is being produced out an even curface in circular sample groove, and its thickness and width meet the condition of test needs.As can be seen from Figure 1, material structure is complete, and inclusion-free exists mutually.
Fig. 2 is the Li of example 1 of the present invention preparation 2ruO 3the electromicroscopic photograph of powdered material, demonstrates this material and is of a size of about 2 μm.
By the Li that embodiment 1 prepares 2ruO 3material, acetylene black and PVDF (polyvinylidene difluoride (PVDF)) are mixed into slurry according to the ratio of mass ratio 8:1:1, afterwards by obtained slurry even application in aluminum substrates, by the electrode slice drying more than 10 hours in vacuum drying oven obtained, pressing treatment is carried out to the electrode slice of drying, then the pole piece of system is cut into size be applicable to thin slice as positive pole, in the glove box being full of argon gas (content of water and oxygen is less than 1PPM) be assembled into experimental cell.The present invention is half-cell to electrode with pure sodium sheet, and the barrier film of battery adopts GLASS MICROFIBER FILTERS GF/C tMbarrier film, electrolytic solution is the organic electrolyte to be dissolved in PC solvent containing 1mol/L sodium perchlorate.Experimental cell carries out charge and discharge cycles test by by computer-controlled auto charge and discharge instrument.
Fig. 3 is the Li of example 1 of the present invention preparation 2ruO 3first three charging and discharging curve of powdered material, as can be seen from Figure 3, initial charge capacity reaches 152.9mAh/g, and specific discharge capacity is close up to 136.6mAh/g. first three specific discharge capacity.
Fig. 4 is the Li of example 1 of the present invention preparation 2ruO 3the charge-discharge performance curve of powdered material, as can be seen from Figure 4, after 50 circulations, charging and discharging capacity is stabilized in about 140mAh/g, and efficiency for charge-discharge, close to 100%, shows good cyclical stability while providing height ratio capacity.
Embodiment 2
Take 0.5mol Li 2cO 3with 0.5mol RuO 2put into agate mortar, add acetone and carry out wet-milling 2 hours, obtain mix powder; Mix powder is carried out compressing tablet, the thin slice of 2 ~ 3mm is pressed into the pressure of 22MPa, be placed in corundum crucible, sinter at the temperature of 900 DEG C in retort furnace, temperature rise rate is 5 DEG C/min, sintering time 24 hours, last naturally cooling, grind into powder afterwards, obtains sodium ion secondary battery positive electrode material Li 2ruO 3.
Positive electrode material embodiment 2 obtained is assembled into experimental cell according to the method for embodiment 1, experimental result shows: to discharge to described battery with the current density of 100mA/g in 2.0 ~ 4.0V voltage range and charge, after 50 circulations, specific discharge capacity is up to 138.2mAh/g.
Embodiment 3
Take 1.5mol Li 2cO 3with 1.5mol RuO 2put into agate mortar, add dehydrated alcohol and carry out wet-milling 2 hours, obtain mix powder; Mix powder is carried out compressing tablet, the thin slice of 2 ~ 3mm is pressed into the pressure of 22MPa, be placed in corundum crucible, sinter at the temperature of 1000 DEG C in retort furnace, temperature rise rate is 5 DEG C/min, sintering time 20 hours, last naturally cooling, grind into powder afterwards, obtains sodium ion secondary battery positive electrode material Li 2ruO 3.
Positive electrode material embodiment 3 obtained is assembled into experimental cell according to the method for embodiment 1, experimental result shows: to discharge to described battery with the current density of 100mA/g in 2.0 ~ 4.0V voltage range and charge, after 50 circulations, specific discharge capacity is up to 141mAh/g.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (8)

1. a sodium ion secondary battery positive electrode material, is characterized in that, the molecular formula of this material is Li 2ruO 3, spacer C2/c.Unit cell parameters: α=90, β=108.5, γ=90.
2. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 1, is characterized in that, comprising:
Step one: by containing the carbonate of lithium and mixing containing the oxide compound of ruthenium, carry out wet-milling, obtain mix powder;
Step 2: mix powder tabletted step one obtained, sinters, and obtains sodium ion secondary battery positive electrode material.
3. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 2, is characterized in that, the described carbonate containing lithium is Li 2cO 3.
4. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 2, is characterized in that, the described oxide compound containing ruthenium is RuO 2.
5. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 2, is characterized in that, the described wet-milling time is 1-2 hour.
6. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 2, is characterized in that, in the described carbonate containing lithium and the oxide compound containing ruthenium, the mol ratio of Li and Ru is 2:1.
7. the preparation method of a kind of sodium ion secondary battery positive electrode material according to claim 2, is characterized in that, the sintering temperature of described step 2 is 900-1000 DEG C, and sintering time is 20-24 hour.
8. the lithium sodium hybrid battery for preparing of sodium ion secondary battery positive electrode material according to claim 1.
CN201410765652.4A 2014-12-12 2014-12-12 Positive electrode material of sodium ion secondary battery, preparation method of positive electrode material, as well as lithium-sodium mixed battery Pending CN104495959A (en)

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WO2024004902A1 (en) * 2022-06-30 2024-01-04 田中貴金属工業株式会社 POSITIVE ELECTRODE ACTIVE MATERIAL FOR Li ION SECONDARY BATTERIES AND METHOD FOR PRODUCING SAME

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Publication number Priority date Publication date Assignee Title
CN114583136A (en) * 2022-03-16 2022-06-03 安徽云储盈鑫有限责任公司 Preparation method of high-performance lithium/sodium ion battery and battery
CN114583136B (en) * 2022-03-16 2024-01-26 安徽云储盈鑫有限责任公司 Preparation method of high-performance lithium/sodium ion battery and battery
WO2024004902A1 (en) * 2022-06-30 2024-01-04 田中貴金属工業株式会社 POSITIVE ELECTRODE ACTIVE MATERIAL FOR Li ION SECONDARY BATTERIES AND METHOD FOR PRODUCING SAME

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Application publication date: 20150408