CN104409713B - Novel lithium ion battery anode material and preparation method thereof - Google Patents
Novel lithium ion battery anode material and preparation method thereof Download PDFInfo
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- CN104409713B CN104409713B CN201410644407.8A CN201410644407A CN104409713B CN 104409713 B CN104409713 B CN 104409713B CN 201410644407 A CN201410644407 A CN 201410644407A CN 104409713 B CN104409713 B CN 104409713B
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- lithium ion
- ion battery
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- sodium carbonate
- sodium
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000010405 anode material Substances 0.000 title abstract 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910020700 Na3VO4 Inorganic materials 0.000 claims abstract description 15
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical group [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000000843 powder Substances 0.000 claims abstract 2
- 239000000126 substance Substances 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 32
- 239000011734 sodium Substances 0.000 claims description 20
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 8
- 230000004087 circulation Effects 0.000 claims description 7
- 239000010406 cathode material Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims 1
- 238000001354 calcination Methods 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000000376 reactant Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- VQBIMXHWYSRDLF-UHFFFAOYSA-M sodium;azane;hydrogen carbonate Chemical compound [NH4+].[Na+].[O-]C([O-])=O VQBIMXHWYSRDLF-UHFFFAOYSA-M 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910011312 Li3VO4 Inorganic materials 0.000 description 2
- 229910003206 NH4VO3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- WGRULTCAYDOGQK-UHFFFAOYSA-M sodium;sodium;hydroxide Chemical compound [OH-].[Na].[Na+] WGRULTCAYDOGQK-UHFFFAOYSA-M 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- -1 vanadium metal oxides Chemical class 0.000 description 1
Classifications
-
- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
A provided novel lithium ion battery anode material has the chemical composition of Na3VO4. A preparation method of the novel lithium ion battery anode material comprises the steps: respectively grinding sodium carbonate and ammonium metavanadate to 1200 mesh, and fully mixing sodium carbonate and ammonium metavanadate according to the sodium-to-vanadium molar ratio of 2.5-3:1 to prepare a powder, and calcining the mixed powder at 450 DEG C-600 DEG C for 5-10 h. Sodium carbonate can be replaced by sodium hydroxide, and ammonium metavanadate can be replaced by vanadium pentoxide. The synthetic method is simple, low in equipment requirement and easy to operate. Reactant kinds demanded by synthesis are less, the raw materials are cheap and easy to obtain, and the prepared sample is uniform in dimension and has the average particle size of about 500 nm. The first charge and discharge capacities of Na3VO4 are respectively 363 and 664.3 mAh/g, and the charge and discharge capacities after 50 times of cycles are 205.5 and 205.9 mAh/g.
Description
Technical field
The present invention relates to a kind of novel cathode material for lithium ion battery, particularly to a kind of Na of solid phase calcination preparation3VO4
Negative material, belongs to field of electrochemical power source.
Background technology
Lithium ion battery is the third generation small battery after nickel-cadmium cell, Ni-MH battery, and because of it, to have energy close
Degree is big, and output voltage is high, and self discharge is little, memory-less effect, operating temperature range width（- 20 DEG C～60 DEG C）, cycle performance is superior,
Can fast charging and discharging, output power, become the representative of modern high performance battery the advantages of long service life.And wherein negative pole
Material is the important component part of lithium ion battery, and the quality of negative material performance directly influences the performance of lithium ion battery.
At present, the research to lithium ion battery negative material, is concentrated mainly on material with carbon element, alloy material and new with lithium titanate as representative
The aspects such as type negative material.Among these, material with carbon element is to be studied and be applied to the business-like material of lithium ion battery earliest by people
Material, is still one of the emphasis of everybody concern and research so far.But the intercalation potential of graphite is relatively low, formed in charge and discharge process
Li dendrite can cause potential safety hazard.The lithium titanate of spinel structure has flat charge and discharge platform at 1.55 V, far above lithium
Dendrite deposition potential, has the security performance being obviously improved as lithium ion battery negative.In addition, lithium titanate has " zero strain "
Feature, this " zero strain " is it can be avoided that lead to structural damage due to stretching back and forth of electrode material, thus improving electricity
The cycle performance of pole and service life, reduce the special capacity fade that circulation brings.But although lithium titanate has and has extended cycle life,
The advantage of high stability, but its specific capacity is low, and theoretical capacity is 175 mAh/g, and actual capacity is generally 160 mAh/g.
Early-stage Study shows new Li3VO4Material shows higher capacity as the Typical Representative of vanadium metal oxides
And preferable cyclical stability, it is a kind of lithium ion battery negative material of great potential.But lithium resource reserves are limited, and cost
Higher, it is unfavorable for Li3VO4The commercialization of electrode material.Through research, we find new Na first3VO4Negative material also has
Higher theoretical specific capacity and stable cycle performance, simultaneously sodium element be widely distributed in a salt form in land and ocean
Rich reserves, cheap.Currently, with respect to Na3VO4As the correlative study of lithium ion battery negative material, there is not been reported.Base
In above research background, the present invention relates to one kind prepares new Na3VO4The method of negative material, and it is used as lithium ion first
Cell negative electrode material.
Content of the invention
The purpose of the present invention is prepared newly with sodium carbonate or NaOH and vanadic anhydride or ammonium metavanadate for precursor
Type lithium ion battery negative material Na3VO4.Na involved in the present invention3VO4Synthesis material be sodium carbonate and vanadic anhydride or
Ammonium metavanadate, during solid phase reaction occur reaction be：
3Na2CO3+V2O5→2Na3VO4+3CO2↑
Or 3Na2CO3+NH4VO3→2Na3VO4+3CO2↑+2NH3↑+H2O
6NaOH+V2O5→2Na3VO4+3H2O
Or 3NaOH+NH4VO3→Na3VO4+NH3↑+2H2O
Comprise the following steps that：
1) will be selected from one of sodium carbonate or NaOH sodium source, in vanadic anhydride or ammonium metavanadate
Plant vanadium source, sodium source will be weighed and vanadium source is ground to 1200 mesh respectively.
2) sodium source after to grind and vanadium source, as raw material, are 2.5 ~ 3 by the mol ratio of sodium and vanadium:1 is sufficiently mixed.
3) take step 2）In mixed powder be contained in material boat, by material boat be placed at 450 DEG C ~ 600 DEG C in stove calcining 5 ~
10h.Material preparation method involved in the present invention and Na3VO4Electrode material has following outstanding feature：
（1）Synthetic method is simple, low for equipment requirements it is easy to operation；
（2）Reactant species required for synthesis are few and raw material prepared sample size cheap and easy to get is uniform, and particle is average
Particle diameter is 500 nm；
（3）Na3VO4Charge and discharge capacity is respectively 363,664.3mAh/g first, and after 50 circulations, charge and discharge capacity is
205.5、205.9mAh/g.
Brief description：
Na prepared by Fig. 1 embodiment 13VO4XRD spectrum.
Na prepared by Fig. 2 embodiment 13VO4SEM figure.
Na prepared by Fig. 3 embodiment 13VO4First charge-discharge curve (a) and cycle performance figure (b).
Na prepared by Fig. 4 embodiment 23VO4XRD spectrum.
Na prepared by Fig. 5 embodiment 23VO4First charge-discharge curve (a) and cycle performance figure (b).
Specific embodiment：
Embodiment 1
Materials synthesis step is as follows：
1) by sodium carbonate, vanadic anhydride, respectively weigh 5g, the sodium carbonate weighing, vanadic anhydride are ground to respectively
1200 mesh.
2) sodium carbonate after to grind and vanadic anhydride press sodium, vanadium mol ratio for 2.5 ~ 3:1 is sufficiently mixed and grinds.
3) take step 2）In mixed powder be contained in material boat, material boat is placed at 550 DEG C in stove calcining 5h.By institute
The Na of preparation3VO4Sample carries out XRD test, as shown in Fig. 1.Result shows, prepared sample is relatively through XRD analysis of spectrum
Pure Na3VO4, corresponding to XRD card JCPDS, no. 27-0827.Fig. 2 is the SEM figure of prepared sample, can from figure
Go out, prepared Na3VO4Pattern be graininess, mean particle size is 500 nm.The material of embodiment 1 gained is pressed
Following method makes battery：The Na that will be obtained3VO4Sample and acetylene black and Kynoar are by weight for 8:1:1 ratio is mixed
Close, slurry is made for solvent with N- first class pyrrolidones, is coated on the Copper Foil of 10 μ m thick, after being dried 10 at 60 DEG C, punching
Become the disk of 14mm, be vacuum dried 12h at 120 DEG C.It is to electrode with metal lithium sheet, Celgard film is barrier film, is dissolved with
LiPF6(1mol/L) (volume ratio is 1 to EC+DMC+DEC:1:1) solution is electrolyte, in the glove box of argon gas protection
It is assembled into CR2025 type battery.Battery pack stands 8h after installing, then carries out constant current charge-discharge survey with CT2001A battery test system
Examination, test voltage is 3 ~ 0.02V.Fig. 3 is prepared Na3VO4Particle shows first as lithium ion battery negative material
Charge and discharge specific capacity be respectively 363,664.3mAh/g, 50 times circulation after charge and discharge specific capacity be respectively 205.5,
205.9mAh/g it is shown that good stable circulation performance.
Embodiment 2
Materials synthesis step is as follows：
1) by sodium carbonate, ammonium metavanadate, respectively weigh 5g, the sodium carbonate weighing, ammonium metavanadate are ground to 1200 respectively
Mesh.
2) sodium source after to grind and vanadium source, as raw material, are 2.5 ~ 3 by the mol ratio of sodium and vanadium:1 is sufficiently mixed.3) take
Step 2）In mixed powder be contained in material boat, material boat is placed at 550 DEG C in stove calcining 5h.By prepared Na3VO4Sample
Product carry out XRD test, as shown in Fig. 4.Result shows, prepared sample is Na through XRD analysis of spectrum3VO4, corresponding to XRD
Card JCPDS, No. 27-0827, containing partial impurities；As described in embodiment 1, step and operation assembled battery are tested, and survey
The Na prepared by embodiment 2 obtaining3VO4The charge and discharge specific volume first that particle shows as Fig. 5 as lithium ion battery negative material
Amount is respectively 319.8,602.1mAh/g, and after 70 circulations, charge and discharge specific capacity is respectively 162.2,163.3mAh/g, display
Preferable stable circulation performance.
Claims (1)
1. a kind of preparation method of novel cathode material for lithium ion battery, the chemical composition of this negative material is Na3VO4, its feature
It is：(1) by sodium carbonate or NaOH, after ammonium metavanadate or vanadic anhydride are ground to 1200 mesh respectively, by sodium and vanadium
Mol ratio is 2.5 ~ 3：1 is sufficiently mixed prepared powder；(2) take mixed powder in step (1) to be contained in material boat, material boat is put
In stove, sintering atmosphere is air, calcines 5 ~ 10h at 450 DEG C ~ 600 DEG C；
Prepared Na3VO4Pattern be graininess, mean particle size be 500 nm, Na3VO4Particle is as lithium ion battery
The specific capacity of charge and discharge first that negative material shows is respectively 363,664.3mAh/g, charge and discharge specific capacity after 50 circulations
It is respectively 205.5,205.9mAh/g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410644407.8A CN104409713B (en) | 2014-11-14 | 2014-11-14 | Novel lithium ion battery anode material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410644407.8A CN104409713B (en) | 2014-11-14 | 2014-11-14 | Novel lithium ion battery anode material and preparation method thereof |
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| CN104409713A CN104409713A (en) | 2015-03-11 |
| CN104409713B true CN104409713B (en) | 2017-02-22 |
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| CN110459735B (en) * | 2018-05-07 | 2021-05-18 | 宁德新能源科技有限公司 | Cathode material, preparation method thereof, battery cathode and lithium ion battery |
| CN115092959B (en) * | 2022-06-16 | 2024-03-26 | 西安理工大学 | Manganese/sodium vanadate material prepared by salt template-assisted solid-phase sintering method, and preparation method and application thereof |
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| CN103496741B (en) * | 2013-09-25 | 2015-12-23 | 三峡大学 | A kind of solid phase reaction method prepares Li 3vO 4negative material |
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