CN104505510A - Negative electrode material of sodium ion secondary batter, preparation method of negative electrode material, as well as sodium ion battery - Google Patents
Negative electrode material of sodium ion secondary batter, preparation method of negative electrode material, as well as sodium ion battery Download PDFInfo
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- CN104505510A CN104505510A CN201410765627.6A CN201410765627A CN104505510A CN 104505510 A CN104505510 A CN 104505510A CN 201410765627 A CN201410765627 A CN 201410765627A CN 104505510 A CN104505510 A CN 104505510A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
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Abstract
The invention provides a negative electrode material of a sodium ion secondary battery, belongs to the technical field of sodium ion secondary battery materials, and solves the problem that the circulating performance of an existing negative electrode material of the sodium ion battery is poor. The molecular formula of the material is Na3V2(PO4)3. The invention further provides a preparation method of the negative electrode material of the sodium ion secondary battery. The invention further provides the sodium ion secondary battery prepared from the negative electrode material of the sodium ion secondary battery. The sodium ion battery adopts the negative electrode material provided by the invention, so that the sodium ion battery has the good electrochemical performance and safety performance; an experiment result shows that, in the first time, the charging specific capacity can be up to 224.9mAh/g, and the discharging specific capacity is up to 125.8mAh/g; and the specific capacity is stabilized to be about 139mAg/g after 50 times of cycles.
Description
Technical field
The invention belongs to sodium ion secondary battery field of material technology, be specifically related to a kind of sodium ion secondary battery negative material, preparation method and sodium-ion battery.
Background technology
In the face of the problem of increasingly serious environmental pollution and energy scarcity, people have promoted the development of stored energy and conversion equipment while probing into novel green alternative energy source, lithium ion battery relies on its higher operating voltage and energy density, good cycle performance, memory-less effect, becomes the study hotspot becoming vast researcher without the outstanding advantages such as self discharge and environmental protection, and starts to be widely used in the small electrical equipment for gasification such as mobile phone, notebook computer, electric motor car.But elemental lithium is only 17 ~ 20 μ about g/g in the memory space of the earth, and by the end of the year 2009, the lithium resource of about 1/4th is used to battery process in the world, and for lithium carbonate, its cost price has reached 5000 dollars per ton.And lithium ion battery more allows people attempt the application of lithium-ion battery system to extend to above large-scale energy-storage system in the successful Application of small electrical equipment for gasification, this industrial production demand to lithium-containing compound that will certainly increase severely, and the memory space of the lithium not enough massive energy storage device meeting the whole world far away, extensive research and development low consumption, high performance lithium-ion electric pool process certainly will be hindered, and memory space that sodium enriches with it, cheap development cost, good performance become the excellent selection of lithium ion battery substituting battery system.
Along with people increase day by day to the demand of extensive energy storing device, the research and development of sodium ion secondary battery electrode material become one of study hotspot in recent years.Sodium ion secondary battery have extremely similar operation principle to lithium ion battery, all using electroactive substance as work electrode.Probe into suitable electrode material also to become people and seek new breakthrough in sodium-ion battery system and be badly in need of a difficult problem of capturing, the sodium-ion battery usually probed into adopts sodium sheet and active material to assemble respectively as positive and negative pole material, and compounds containing sodium is Na such as
xcoO
2, NaFeF
3, NaTi
2(PO
4)
3, Na
4mn
9o
18, Na
1.5vOPO
4f
0.5, NaCrO
2, Na
2ti
3o
7, Na
xvO
2, Na
2fePO
4f, NaMPO
4deng being carried out electro-chemical test as positive electrode.But go no further relative to the Exploration and Research of anode material of lithium-ion battery always, probe into that a kind of to have outstanding macrocyclic negative material most important for the development of sodium-ion battery system.The people such as Zelang Jian in 2012 pass through the coated Na of Solid phase synthesis carbon
3v
2(PO
4)
3test as sodium-ion battery positive material under 2.7-3.8V, its first charge-discharge capacity reaches 98.6/93mAh/g, and after ten circulations, capacity can remain on 99%, and cycle performance is excellent, Na
3v
2(PO
4)
3have these two discharge platforms of 1.6V and 3.38V, its theoretical capacity in the scope of 118mAh/g ~ 236mAh/g, at present also not by Na
3v
2(PO
4)
3as the report of negative material application with sodium-ion battery.
Summary of the invention
The object of the invention is the problem of the negative material cycle performance difference in order to solve existing sodium-ion battery, and a kind of sodium ion secondary battery negative material, preparation method and sodium-ion battery are provided.
First the present invention provides a kind of sodium ion secondary battery negative material, and the molecular formula of this material is Na
3v
2(PO
4)
3, have
space group, has sodium fast ion conduction (NASICON) structure, cell parameter
two VO
6be connected in the Z-axis direction with three phosphates and form basic support, sodium ion is positioned at 6b and the 18b position of standoff gap.
The present invention also provides a kind of preparation method of anode material of lithium-ion battery, comprising:
Step one: be dissolved in citric acid solution by sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate, carries out stirring reaction in alkali lye, obtains mixture gel;
Step 2: mixture gel abrasive step one obtained becomes powder, obtains mix powder, by mix powder presintering, obtains mixture precursor;
Step 3: mixture precursor tabletted step 2 obtained, sinters, obtain anode material of lithium-ion battery.
Preferably, the mol ratio of described sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate is 3:6:4.
Preferably, the temperature of the presintering of described step 2 is 350 DEG C ~ 400 DEG C, and the time is 5 ~ 7 hours.
Preferably, described mixture precursor is tabletted under 18-22MPa.
Preferably, the sintering temperature of described step 3 is 650 DEG C ~ 800 DEG C, and sintering time is 12 ~ 15 hours.
Present invention also offers the sodium-ion battery that above-mentioned anode material of lithium-ion battery prepares.
Beneficial effect of the present invention
First the present invention provides a kind of sodium ion secondary battery negative material, and its molecular formula is Na
3v
2(PO
4)
3, the present invention is first by Na
3v
2(PO
4)
3use as negative material, and this lower cost for material, have with battery prepared by this material that security performance is high, the advantage of stable cycle performance.
The present invention also provides a kind of preparation method of sodium ion secondary battery negative material, and the method is dissolved in citric acid solution by sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate, in alkali lye, carry out stirring reaction, obtains mixture gel; Then mixture gel abrasive is become powder, obtain mix powder, by mix powder presintering, obtain mixture precursor; Mixture precursor tabletted will be walked again, sinter, obtain anode material of lithium-ion battery.Compare with prior art, sintering time of the present invention is shorter, and preparation method is simple, cost is lower, is applicable to large-scale industrial production.
The sodium ion secondary battery that the present invention also provides a kind of above-mentioned sodium ion secondary battery negative material to prepare, this sodium-ion battery is owing to have employed negative material of the present invention, this sodium-ion battery has good chemical property and security performance, experimental result shows: initial charge specific capacity can reach 224.9mAh/g, specific discharge capacity reaches 125.8mAh/g, and its specific capacity that circulates for 50 times can be stabilized in about 139mAh/g.
Accompanying drawing explanation
Fig. 1 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3the X ray diffracting spectrum of dusty material.
Fig. 2 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3dusty material is as the charge-discharge performance curve of negative material.
Fig. 3 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3dusty material and the high rate performance test curve as negative material.
Fig. 4 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3dusty material and as negative material cyclic curve of 1000 times under the current density of 1A/g.
Embodiment
First the present invention provides a kind of sodium ion secondary battery negative material, and its molecular formula is Na
3v
2(PO
4)
3, have
space group, has sodium fast ion conduction (NASICON) structure, cell parameter
two VO
6be connected in the Z-axis direction with three phosphates and form basic support, sodium ion is positioned at 6b and the 18b position of standoff gap.This material of wider voltage range has 1.6V and 3.4V two discharge platforms, correspond to V respectively
2+/ V
3+and V
3+/ V
4+redox reaction, two sodium ions can be had to carry out deintercalation behavior, and theoretical capacity is between 118mAh/g ~ 236mAh/g.
The present invention also provides a kind of preparation method of anode material of lithium-ion battery, comprising:
Step one: be dissolved in citric acid solution by sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate, carries out stirring reaction in alkali lye, obtains mixture gel;
Step 2: mixture gel abrasive step one obtained becomes powder, obtains mix powder, by mix powder presintering, obtains mixture precursor;
Step 3: mixture precursor tabletted step 2 obtained, sinters, obtain anode material of lithium-ion battery.
According to the present invention, described in step one with sodium carbonate (Na
2cO
3), ammonium hydrogen phosphate (NH
4h
2pO
4), ammonium metavanadate (NH
4vO
3) for raw material is dissolved in citric acid solution, the concentration of described citric acid solution is preferably 0.02mol/L, described sodium carbonate (Na
2cO
3), ammonium hydrogen phosphate (NH
4h
2pO
4), ammonium metavanadate (NH
4vO
3) mol ratio be preferably 3:6:4, preferably, in the alkali lye of pH=9 at constant temperature 70 DEG C ~ 80 DEG C stir until mixed solution gel in the pasty state, obtain mixture gel.
According to the present invention; the above-mentioned mixture gel that obtains is dried; pulverize; described bake out temperature is preferably 80 DEG C ~ 100 DEG C; drying time is preferably 10 ~ 12 hours, the mixed-powder obtained preferably is carried out presintering under nitrogen protection, obtains mixture precursor; pre-sintering temperature preferably 350 DEG C ~ 400 DEG C, the time is 5 ~ 7 hours.
According to the present invention, by said mixture precursor preferably tabletted under 18-22MPa, preferably sinter under nitrogen protection, obtain anode material of lithium-ion battery.Described sintering temperature is preferably 650 DEG C ~ 800 DEG C, and sintering time is preferably 12 ~ 15 hours.
The sodium-ion battery that the present invention also provides above-mentioned sodium ion secondary battery negative material to prepare.The preparation method of sodium-ion battery of the present invention is the technical method that this area is commonly used, and is not particularly limited, preferably includes: by the Na prepared
3v
2(PO
4)
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 Na of the present invention
3v
2(PO
4)
3material, acetylene black and PVDF (Kynoar) are mixed into slurry according to the ratio of mass ratio 7:2:1, afterwards by obtained slurry even application on substrate, by the electrode slice drying more than 10 hours in vacuum drying oven obtained, compression process 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 electrode, 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, electrolyte 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 oxide spinel sodium related in embodiment, ammonium hydrogen phosphate, ammonium metavanadate are respectively Beijing Chemical Plant and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Embodiment 1
By 0.003mol sodium carbonate, 0.006mol ammonium hydrogen phosphate and 0.004mol ammonium metavanadate are dissolved in the citric acid solution of the 0.02mol/L of 100ml, thermal agitation is added until solution presents pastes gels at constant temperature 70 DEG C under the alkalescent liquid environment of PH=9, obtain mixture gel, then drying box mixture gel being put into 80 DEG C grinds to form mix powder at agate mortar after dry 10 hours, 7 hours are incubated after mix powder is pre-sintered to 350 DEG C under nitrogen protection, naturally take out after cooling, obtain mixture precursor, mixture precursor is made sheet at the pressure of 22MPa, sheet presoma is sintered to 650 DEG C under nitrogen protection and is incubated 15 hours and naturally cool rear taking-up, obtain sodium ion secondary battery negative material.
Fig. 1 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3x-ray diffraction (XRD) collection of illustrative plates of dusty 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.Carry out indexing to the XRD collection of illustrative plates obtained, the sample powder obtained as seen from Figure 1 is pure phase.
Sodium ion secondary battery negative material embodiment 1 obtained, acetylene black and PVDF (Kynoar) are mixed into slurry according to the ratio of 7:2:1, and even application is on Copper Foil substrate.After the electrode slice obtained is dried 10 hours in the vacuum drying oven of 120 DEG C, tight at 20MPa pressure, then the pole piece of system is cut into the thin slice that is of a size of 8mm × 8mm as electrode (active material containing about 1.7mg on each thin slice), being half-cell with pure sodium sheet, (diameter is for about 1cm to electrode, thickness is the disk of about 3mm), with the sodium perchlorate containing 1mol/L for solute, PC be solvent configuration organic liquid be electrolyte, in the glove box being full of argon gas (content of water and oxygen is less than 1PPM) be assembled into experimental cell.By Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3dusty material is tested under the voltage range of 0.01 ~ 3.0V as negative material, and its initial charge specific capacity can reach 224.9mAh/g, and specific discharge capacity reaches 125.8mAh/g, and its specific capacity that circulates for 50 times can be stabilized in about 139mAh/g, and Fig. 2 is Na
3v
2(PO
4)
3dusty material is as the charge-discharge performance curve of negative material, and Fig. 3 is Na prepared by the embodiment of the present invention 1
3v
2(PO
4)
3the high rate performance curve chart of dusty material, under 2A/g, its capacity still can reach about 60mAh/g.Fig. 4 is Na
3v
2(PO
4)
3dusty material is at the cyclic curve of 1A/g current density 1000 times, and after 1000 circulations, its specific capacity can reach 67.5mAh/g, and capability retention is 75.6%.Na prepared by the embodiment of the present invention 1 can be found out from Fig. 3 and Fig. 4
3v
2(PO
4)
3dusty material not only has excellent high rate performance, and under high magnification, show remarkable cycle performance.
Embodiment 2
By 0.0015mol sodium carbonate, 0.003mol ammonium hydrogen phosphate and 0.002mol ammonium metavanadate are dissolved in the citric acid solution of the 0.02mol/L of 50ml, thermal agitation is added until solution presents pastes gels at constant temperature 80 DEG C under the alkalescent liquid environment of PH=9, obtain mixture gel, then drying box mixture gel being put into 90 DEG C grinds to form mix powder at agate mortar after dry 11 hours, 6 hours are incubated after mix powder is pre-sintered to 400 DEG C under nitrogen protection, naturally take out after cooling, obtain mixture precursor, mixture precursor is made sheet at the pressure of 22MPa, sheet presoma is sintered to 750 DEG C under nitrogen protection and is incubated 14 hours and naturally cool rear taking-up, obtain sodium ion secondary battery negative material.
Sodium ion secondary battery electrode material embodiment 2 obtained is assembled into battery according to the method for embodiment 1, experimental result shows: with discharge and recharge under the current density of 200mA/g under 0.01V ~ 3V voltage range, and its specific capacity is stabilized in 100mAh/g and does not decay after 500 circulations.
Embodiment 3
By 0.006mol sodium carbonate, 0.012mol ammonium hydrogen phosphate and 0.008mol ammonium metavanadate are dissolved in the citric acid solution of the 0.02mol/L of 200ml, thermal agitation is added until solution presents pastes gels at constant temperature 80 DEG C under the alkalescent liquid environment of PH=9, obtain mixture gel, then drying box mixture gel being put into 100 DEG C grinds to form mixed-powder thing at agate mortar after dry 12 hours, 5 hours are incubated after mix powder is pre-sintered to 400 DEG C under nitrogen protection, naturally take out after cooling, obtain mixture precursor, mixture precursor is made sheet at the pressure of 22MPa, sheet presoma is sintered to 800 DEG C under nitrogen protection and is incubated 12 hours and naturally cool rear taking-up, obtain sodium ion secondary battery electrode material.
Sodium ion secondary battery electrode material embodiment 3 obtained is assembled into battery according to the method for embodiment 1, experimental result shows: with discharge and recharge under the current density of 2A/g under 0.01V ~ 3V voltage range, and its first charge-discharge specific capacity can reach 60mAh/g and after 3000 circulations, specific capacity can remain on about 40mAh/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 range 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 negative material, is characterized in that, the molecular formula of this material is Na
3v
2(PO
4)
3, have
space group, has sodium fast ion conduction (NASICON) structure, cell parameter
two VO
6be connected in the Z-axis direction with three phosphates and form basic support, sodium ion is positioned at 6b and the 18b position of standoff gap.
2. the preparation method of a kind of anode material of lithium-ion battery according to claim 1, is characterized in that, comprising:
Step one: be dissolved in citric acid solution by sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate, carries out stirring reaction in alkali lye, obtains mixture gel;
Step 2: mixture gel abrasive step one obtained becomes powder, obtains mix powder, by mix powder presintering, obtains mixture precursor;
Step 3: mixture precursor tabletted step 2 obtained, sinters, obtain anode material of lithium-ion battery.
3. the preparation method of a kind of anode material of lithium-ion battery according to claim 2, is characterized in that, the mol ratio of described sodium carbonate, ammonium hydrogen phosphate and ammonium metavanadate is 3:6:4.
4. the preparation method of a kind of anode material of lithium-ion battery according to claim 2, is characterized in that, the reaction temperature of described step one is 70-80 DEG C.
5. the preparation method of a kind of anode material of lithium-ion battery according to claim 2, is characterized in that, the temperature of the presintering of described step 2 is 350 DEG C ~ 400 DEG C, and the time is 5 ~ 7 hours.
6. the preparation method of a kind of anode material of lithium-ion battery according to claim 2, is characterized in that, described mixture precursor is tabletted under 18-22MPa.
7. the preparation method of a kind of anode material of lithium-ion battery according to claim 2, is characterized in that, the sintering temperature of described step 3 is 650 DEG C ~ 800 DEG C, and sintering time is 12 ~ 15 hours.
8. the sodium-ion battery for preparing of anode material of lithium-ion battery according to claim 1.
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| CN105702956A (en) * | 2015-12-28 | 2016-06-22 | 上海电力学院 | Negative material for sodium-ion battery and preparation method of negative material |
| CN106848288A (en) * | 2017-01-20 | 2017-06-13 | 东莞市迈科新能源有限公司 | A kind of sodium-ion battery positive material of La doped and preparation method thereof |
| CN107123809A (en) * | 2017-04-07 | 2017-09-01 | 武汉理工大学 | The production method of vanadium phosphate sodium reference symmetry type high voltage sodium ion secondary battery |
| CN107720718A (en) * | 2017-09-12 | 2018-02-23 | 华中科技大学 | A kind of high voltage N ASICON structures water system sodium-ion battery negative material and its synthetic method |
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