CN107611420B - Lithium battery nano electrode material LiNaV2O6And method for preparing the same - Google Patents
Lithium battery nano electrode material LiNaV2O6And method for preparing the same Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 30
- 239000007772 electrode material Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 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 abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 239000011858 nanopowder Substances 0.000 claims abstract description 3
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 12
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 11
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 239000010405 anode material Substances 0.000 abstract description 3
- 238000012719 thermal polymerization Methods 0.000 abstract description 3
- 238000010668 complexation reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract 1
- 229910012985 LiVO3 Inorganic materials 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000010406 cathode material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910012970 LiV3O8 Inorganic materials 0.000 description 1
- 229910019501 NaVO3 Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a lithium battery nano electrode material LiNaV2O6And a process for the preparation thereof, which process comprisesThe following steps: adding a lithium source, a sodium source and a vanadium source into an acrylic acid aqueous solution according to the molar ratio of elements in the molecular formula, adding an acid to adjust the pH value to form a stable aqueous solution, performing thermal polymerization to form gel dry powder, grinding and performing heat treatment on the obtained dry powder to obtain a nano powder material LiNaV2O6. According to the invention, a wet chemical method is adopted to realize the full mixing of different raw materials, the V element is stabilized through an acrylic acid complexation reaction, a xerogel is formed by utilizing the thermal polymerization of acrylic acid to inhibit the particle growth in the heat treatment process, and the nanometer material is simply and effectively prepared; na having a larger ion radius+Introduced into a laminated structure to realize LiNaV2O6The lithium ion transmission rate and the structural stability of the material are improved; when the material is used as a lithium battery anode material, the gram volume is high, and the cycle performance and the rate performance are good; meanwhile, the method has the advantages of simple preparation process, short preparation period, high efficiency and the like.
Description
Technical Field
The invention relates to the field of lithium battery materials, in particular to a lithium battery nano electrode material LiNaV2O6And a method for preparing the same.
Background
With the increasing demand for energy, the exploration of new energy storage devices and energy storage materials with excellent performance has become one of the hot spots in the development of current technologies. Among them, lithium batteries have gained wide attention and rapid development because of their advantages such as higher energy density, longer cycle life, no memory effect, higher safety, and good environmental protection. Among the many key components of lithium batteries, the positive electrode material is an important factor affecting the energy density, power density, cycle life, and safety performance of the battery, and is the most critical component of the lithium battery. Among them, the cathode material having a layered structure is a commonly used cathode material due to its good structural stability and high lithium ion transmission rate, such as layered lithium cobaltate and ternary materials, which are widely used. However, in such materials, the disadvantages of low gram-capacity, low energy density, scarce resources, high cost and the like are commonly existed.
Compared with the prior commonly used layered cathode material, the layered structure vanadium cathode material such as V2O5、LiVO3And LiV3O8Also has rich vanadium resource, simple synthesis process, low cost and high gram volumeAnd the lithium ion battery has the advantages of high energy density and the like, and is a relatively ideal lithium battery anode material. However, with the increase of the lithium ion intercalation amount in the charging and discharging processes, the layered structure of the material can generate disorder and irreversible phase change, which causes the reduction of gram capacity and cycle performance attenuation of the material and limits the application of the material.
Disclosure of Invention
The invention aims to provide a lithium battery nano electrode material LiNaV2O6The material has the advantages of high structural stability and lithium ion conductivity, simple preparation process, short preparation period and high efficiency.
The purpose of the invention can be realized by the following technical scheme:
lithium battery nano electrode material LiNaV2O6The preparation method comprises the following steps:
(1) according to LiNaV2O6Adding a lithium source, a sodium source and a vanadium source into an aqueous solution of acrylic acid, and adding an acid to adjust the pH value to form a stable aqueous solution;
(2) heating the aqueous solution obtained in the step (1) to T1, and preserving heat to enable the aqueous solution to form gel and dry the gel into fluffy dry powder;
(3) grinding the dry powder obtained in the step (2), heating to the temperature T2 for heat treatment reaction to obtain a nano powder material LiNaV2O6。
Preferably, the lithium source in step (1) is one or more selected from lithium acetate, lithium nitrate and lithium hydroxide.
Preferably, the sodium source in step (1) is selected from one or more of sodium acetate, sodium nitrate, sodium carbonate, sodium hydroxide, sodium metavanadate and sodium vanadate.
Preferably, the vanadium source in step (1) is selected from one or more of ammonium metavanadate, vanadium pentoxide, sodium metavanadate and sodium vanadate.
Preferably, the pH adjusting acid in step (1) is one or more selected from nitric acid, hydrochloric acid, oxalic acid, citric acid and tartaric acid.
Preferably, the molar concentration of vanadium ions in the aqueous solution in the step (1) is not higher than 0.3 mol/L, the molar ratio of vanadium ions to acrylic acid is not higher than 1, and the pH value of the aqueous solution is not higher than 2.5.
Preferably, the heat preservation temperature T1 in the step (2) is 80-200 ℃, and the heat preservation time is 1.5-48 h.
Preferably, the sintering heat preservation temperature T2 in the step (3) is 300-600 ℃, and the heat treatment time is 6-24 h.
The invention also aims to provide a lithium battery nano-electrode material LiNaV prepared by the method2O6。
The invention has the beneficial effects that: the invention passes Na with larger ionic radius+Substitution of Li having a smaller ionic radius+The lithium ion transmission channel in the layered structure can be expanded, which is beneficial to improving the lithium ion transmission rate of the material; na element and Li element are adjacent elements in the same main group, LiVO3With NaVO3The crystal belongs to a monoclinic system, and the space group is C2/C, so that a stable solid solution can be formed, and the structural stability is improved; the V element is stabilized through acrylic acid complexation, xerogel is formed through acrylic acid thermal polymerization, the growth of nano particles in the heat treatment process is inhibited, and the nano-scale material can be obtained. The invention relates to a nano LiNaV2O6When the material is applied to a lithium battery anode material, the advantage of high gram capacity is kept, the lithium ion transmission rate is high, and the cycle performance and the rate capability of the material can be improved; and the preparation process is simple, the preparation period is short, and the efficiency is high.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Comparative example: weighing raw materials of lithium acetate and vanadium pentoxide according to a molar ratio of 1:1, uniformly mixing by a dry method, heating to 450 ℃ in the air, and preserving heat for 12 hours to obtain LiVO3A material.
Example 1: adding lithium nitrate, sodium nitrate, ammonium metavanadate and acrylic acid into water according to the molar ratio of 1:1:2:4, and dropwise adding 1:3 nitric acid to form an aqueous solution, wherein the pH value of the aqueous solution is 1.5, and the molar concentration of vanadium ions is 0.15 mol/L. The solution is raisedHeating to 150 deg.C, keeping the temperature for 15h to obtain fluffy dry powder, grinding, mixing, and heat treating at 350 deg.C for 10h to obtain nano LiNaV2O6A material.
Example 2: adding lithium acetate, sodium acetate, vanadium pentoxide and acrylic acid into water according to the molar ratio of 1:1:1:3, and dropwise adding 1:2 hydrochloric acid to form an aqueous solution, wherein the pH value of the aqueous solution is 1, and the molar concentration of vanadium ions is 0.1 mol/L. Heating the solution to 180 ℃ and preserving heat for 6h to obtain fluffy dry powder, grinding and mixing the fluffy dry powder, and then carrying out heat treatment for 8h at 450 ℃ to obtain the nano LiNaV2O6A material.
Example 3: adding lithium acetate, sodium metavanadate, vanadium pentoxide and acrylic acid into water according to the mol ratio of 1:1:0.5:2.5, and adding oxalic acid to form an aqueous solution, wherein the pH value of the aqueous solution is 2, and the molar concentration of vanadium ions is 0.15 mol/L. Heating the solution to 100 ℃, preserving the temperature for 15h to obtain fluffy dry powder, grinding and mixing the powder, and then carrying out heat treatment at 300 ℃ for 24h to obtain the nano LiNaV2O6A material.
Example 4: adding lithium hydroxide, sodium vanadate, ammonium metavanadate and acrylic acid into water according to a molar ratio of 3:1:5:6, and adding 1:1 nitric acid to form an aqueous solution, wherein the pH value of the aqueous solution is 1.5, and the molar concentration of vanadium ions is 0.3 mol/L. Heating the solution to 80 deg.C, keeping the temperature for 48h to obtain fluffy dry powder, grinding, mixing, and heat treating at 500 deg.C for 12h to obtain nano LiNaV2O6A material.
Example 5: adding lithium acetate, sodium acetate, ammonium metavanadate and acrylic acid into water according to the molar ratio of 1:1:2:3.5, and adding tartaric acid to form an aqueous solution, wherein the pH value of the aqueous solution is 2.5, and the molar concentration of vanadium ions is 0.05 mol/L. Heating the solution to 200 deg.C, maintaining the temperature for 1.5h to obtain fluffy dry powder, grinding, mixing, and heat treating at 600 deg.C for 6h to obtain nano LiNaV2O6A material.
The particle size of the materials prepared in the comparative examples and examples was characterized by an electron scanning microscope, the lithium ion migration rate by a constant current intermittent titration method (GITT), and the electrochemical performance by a 2016 coin cell test. The button cell manufacturing and testing method comprises the following steps: the pole piece is prepared from active substances: conductive agent acetylene black: and (3) preparing a 2016 button half cell in a glove box filled with argon by using a binder polyvinylidene fluoride (PVDF) as a binder to be 8:1:1 and a lithium sheet as a counter electrode. The charging and discharging interval of the half cell is 1.5-4.0V, and after 3 times of charging and discharging circulation at 0.1C, the circulation performance test at 1C is carried out.
The following table shows the comparison of physical and chemical properties of the materials in each example. It can be seen that LiVO prepared in comparative example3The material particle size is micron-scale with the largest average particle size, while LiNaV prepared with the aid of acrylic acid in the examples2O6The average particle size of the material particles is less than 500 nm. The lithium ion migration rates of various materials were measured by the constant current intermittent titration method (GITT), and it can be seen that the nano-sized LiNaV2O6The lithium ion migration rate of the material is far higher than micron-sized LiVO3A material. The electrochemical test result also shows that the nano-scale LiNaV2O6The 0.1C and 1C discharge specific capacity and the cycle performance of the material are superior to those of micron-sized LiVO3A material.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications can be made to the embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (9)
1. Lithium battery nano electrode material LiNaV2O6The preparation method is characterized by comprising the following steps:
(1) according to LiNaV2O6Adding a lithium source, a sodium source and a vanadium source into an aqueous solution of acrylic acid, and adding an acid to adjust the pH value to form a stable aqueous solution;
(2) heating the aqueous solution obtained in the step (1) to T1, and preserving heat to enable the aqueous solution to form gel and dry the gel into fluffy dry powder;
(3) grinding the dry powder obtained in the step (2), heating to the temperature T2 for heat treatment reaction to obtain a nano powder material LiNaV2O6。
2. The lithium battery nano-electrode material LiNaV according to claim 12O6The preparation method is characterized in that the lithium source in the step (1) is one or more selected from lithium acetate, lithium nitrate and lithium hydroxide.
3. The lithium battery nano-electrode material LiNaV according to claim 12O6The preparation method of (2), wherein the sodium source in step (1) is one or more selected from the group consisting of sodium acetate, sodium nitrate, sodium carbonate, sodium hydroxide, sodium metavanadate and sodium vanadate.
4. The lithium battery nano-electrode material LiNaV according to claim 12O6The preparation method is characterized in that the vanadium source in the step (1) is one or more selected from ammonium metavanadate, vanadium pentoxide, sodium metavanadate and sodium vanadate.
5. The lithium battery nano-electrode material LiNaV according to claim 12O6The method for producing (1), wherein the pH adjusting acid in the step (1) is one or more selected from the group consisting of nitric acid, hydrochloric acid, oxalic acid, citric acid and tartaric acid.
6. The lithium battery nano-electrode material LiNaV according to claim 12O6Characterized in that, in the step (1), the methodThe molar concentration of vanadium ions in the aqueous solution is not higher than 0.3 mol/L, the molar ratio of the vanadium ions to acrylic acid is not higher than 1, and the pH value of the aqueous solution is not higher than 2.5.
7. The lithium battery nano-electrode material LiNaV according to claim 12O6The preparation method is characterized in that the heat preservation temperature T1 in the step (2) is 80-200 ℃, and the heat preservation time is 1.5-48 h.
8. The lithium battery nano-electrode material LiNaV according to claim 12O6The preparation method is characterized in that the temperature T2 in the step (3) is 300-600 ℃, and the heat treatment time is 6-24 h.
9. A lithium battery nano-electrode material LiNaV prepared by the method of claim 12O6。
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| CN1287012C (en) * | 2004-10-26 | 2006-11-29 | 武汉理工大学 | Large scale in situ preparation method of ternary NaV6O15 single crystal nanometer needle |
| CN106192006B (en) * | 2015-05-08 | 2018-03-09 | 中国科学院新疆理化技术研究所 | Compound lithium vanadate sodium optical crystal and its production and use |
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