CN104201363B - The coated Li of a kind of carbon3VO4Lithium ion battery cathode material and its preparation method - Google Patents
The coated Li of a kind of carbon3VO4Lithium ion battery cathode material and its preparation method Download PDFInfo
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- CN104201363B CN104201363B CN201410305710.5A CN201410305710A CN104201363B CN 104201363 B CN104201363 B CN 104201363B CN 201410305710 A CN201410305710 A CN 201410305710A CN 104201363 B CN104201363 B CN 104201363B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010406 cathode material Substances 0.000 title description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 27
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 16
- 229910011312 Li3VO4 Inorganic materials 0.000 claims abstract description 15
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 9
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000012265 solid product Substances 0.000 claims abstract 4
- 239000002994 raw material Substances 0.000 claims abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002105 nanoparticle Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 229910003481 amorphous carbon Inorganic materials 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000004087 circulation Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910009866 Ti5O12 Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- 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
-
- 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 the coated Li of a kind of carbon3VO4Lithium ion battery negative material, this negative material is taking vanadic anhydride, lithium carbonate and hexamethylenetetramine as raw material, phase solution in the middle of obtaining by hydro-thermal reaction, then in the middle of citric acid being joined, in phase solution, mix, oven dry obtains solid product, this solid product is made to amorphous carbon after high-temperature atmosphere sintering and be coated on Li3VO4The lithium ion battery negative material on surface, this negative material is graininess, particle diameter is 90 ~ 120nm. The present invention has utilized the carbonization refinement Li of citric acid3VO4Particle is also evenly coated carbon-coating at particle surface. Synthesis technique is simple, easy operating, and material preparation cost is low. Li in prepared sample3VO4For uniform nano particle, be of a size of 90 ~ 120nm. In gained sample, amorphous carbon is evenly coated on Li3VO4Particle surface. Prepared material charge/discharge capacity is high, cycle performance excellence.
Description
Technical field
The present invention relates to a class new type lithium ion battery composite negative pole material, particularly the coated Li of a kind of carbon3VO4CompoundThe technology of preparing of material and storage lithium characteristic thereof, belong to electrochemistry field of novel.
Background technology
Lithium ion battery has that operating voltage is high, specific energy is large, discharge potential curve is steady, self discharge is little, cycle lifeThe advantages such as long, cryogenic property is good, memoryless, pollution-free, be widely used at present mobile communication equipment as notebook computer andIn mobile phone, also have broad application prospects in as electric automobile and electric bicycle at following electric vehicle. Affect lithiumA key factor of ion battery development is research and development and the application of positive and negative electrode material. Li3VO4As the novel negative pole material of oneMaterial, has more high-volume and capacity ratio and better security performance than commercial graphite negative electrodes material, thanLi4Ti5O12Negative material has higher specific capacity, lower charge and discharge voltage, and current commercial positive electrode couplingWell, in lithium ion battery, have broad application prospects. There are some researches show, by Li3VO4With Graphene is compound can be obviousImprove its capacity and stable circulation performance, but Graphene cost is too high, is unfavorable for extensive preparation. In addition, by Li3VO4Directly heavyAmass and in nickel foam, also effectively improved its chemical property. Prepare the coated Li of carbon by straightforward procedure3VO4Composite construction is expected toImprove Li3VO4Material electrochemical performance, for Li3VO4Practical application in lithium ion battery also has very important meaningJustice. Up to the present, the coated Li of carbon3VO4The research of the preparation of composite construction and the application in lithium ion battery thereof not yet appears in the newspapersRoad. Based on above background, this patent is invented a kind of effective ways and is prepared the coated Li of carbon3VO4Nano particle composite construction, with madeThe coated Li of standby carbon3VO4Composite has shown higher specific capacity and excellent stable circulation as lithium ion battery negativeProperty.
Summary of the invention
Object of the present invention is exactly taking vanadic anhydride, lithium carbonate, hexamethylenetetramine and citric acid as precursor, passes throughHydro-thermal reaction is also coated Li in conjunction with sintered at high temperature New Type of Carbon3VO4Lithium ion battery composite material. First its principle is exactlyUtilize hydro-thermal reaction to prepare precursor solution, then introduce citric acid and fully stir citric acid is mixed all with precursor liquidEven, dry and utilize high-temperature heating that reaction energy is provided, obtain the coated Li of carbon by solid phase reaction3VO4Nano particle composite junctionStructure.
Li involved in the present invention3VO4Synthesis material is vanadic anhydride, lithium carbonate, hexamethylenetetramine and citric acid.In material preparation process, first by vanadic anhydride, lithium carbonate and hexamethylenetetramine by molar ratio 1:3:5: take, placeIn beaker, add appropriate distilled water and stir, be then positioned over and in hydrothermal reaction kettle, at 120 ~ 180 DEG C, react 12 ~ 48 littleTime. The solution that reaction is obtained is transferred in beaker and adds a certain amount of citric acid, after fully stirring, in baking oven, dries,Under condition of nitrogen gas, be heated to eventually at 500 ~ 600 DEG C sintering 2 ~ 10 hours, the naturally cooling coated Li of carbon that obtains3VO4Sample.
The coated Li of carbon involved in the present invention3VO4Negative material and preparation method have following distinguishing feature:
(1) the present invention has utilized the carbonization refinement Li of citric acid3VO4Particle is also evenly coated carbon-coating at particle surface.
(2) synthesis technique is simple, easy operating, and material preparation cost is low.
(3) Li in prepared sample3VO4For uniform nano particle, be of a size of 90 ~ 120nm.
(4) in gained sample, amorphous carbon is evenly coated on Li3VO4Particle surface.
(5) prepared material charge/discharge capacity is high, cycle performance excellence.
Brief description of the drawings
The XRD collection of illustrative plates of Fig. 1 embodiment 1 prepared sample.
The Raman collection of illustrative plates of Fig. 2 embodiment 1 prepared sample.
The SEM figure (a) of Fig. 3 embodiment 1 prepared sample and TEM figure (b).
The curve of charge and discharge first (a) of prepared sample and cycle performance figure (b) (current density 0.1 in Fig. 4 embodiment 1mAcm-2）。
The curve of charge and discharge first (a) of prepared sample and cycle performance figure (b) (current density 0.1 in Fig. 5 embodiment 2mAcm-2）。
The curve of charge and discharge first (a) of prepared sample and cycle performance figure (b) (current density 0.1 in Fig. 6 embodiment 3mAcm-2）。
Detailed description of the invention
Embodiment 1
Take 1mmol vanadic anhydride, 3mmol lithium carbonate and 5mmol hexamethylenetetramine to beaker, add appropriate distillationWater stirs, and is transferred in hydro-thermal axe and reacts 140 degree 24 hours, and reaction gained solution is transferred in beaker and is added0.05mmol citric acid, fully stirs post-drying. Oven dry product is positioned in crucible, and crucible is moved into high temperature process furnancesIn, at 550 DEG C, under condition of nitrogen gas, to calcine 5 hours, the naturally cooling carbon that can obtain is coated Li3VO4Sample. Result shows, madeStandby sample, through XRD atlas analysis, is positioned at 16.3o、21.6o、22.9o、24.4o、28.2o、32.8o、36.3o、37.6o、49.8o、58.7o、66.2oWith 70.9oThe diffraction maximum at place corresponds respectively to rhombic system Li3VO4(XRD card JCPDS, No.38-1247) (100), (110), (011), (101), (111), (200), (002), (201), (202), (320), (203) and(322) crystal face. Prepared sample is through Raman analysis, is positioned at 1358 and 1601cm-1The peak at place derives from carbon. Prepared carbonCoated Li3VO4Composite characterizes through SEM and TEM, can be found out Li by Fig. 3 (a)3VO4For nano particle, average-sizeAbout 100nm. Can be found out by Fig. 3 (b), carbon is evenly coated on Li3VO4Nano grain surface. Coated with prepared carbonLi3VO4Nano particle shows first that as lithium ion battery negative material charge and discharge capacity is 537 and 688mAh/g, 100 timesAfter circulation, charge and discharge capacity is 562 and 565mAh/g, has shown higher specific capacity and excellent stable circulation performance.
Embodiment 2
Take 1mmol vanadic anhydride, 3mmol lithium carbonate and 5mmol hexamethylenetetramine to beaker, add appropriate distillationWater stirs, and is transferred in hydro-thermal axe and reacts 140 degree 24 hours, and reaction gained solution is transferred in beaker and is added0.05mmol citric acid, fully stirs post-drying. Oven dry product is positioned in crucible, and crucible is moved into high temperature process furnancesIn, at 500 DEG C, under condition of nitrogen gas, to calcine 5 hours, the naturally cooling carbon that can obtain is coated Li3VO4Sample. Result shows, with instituteThe coated Li of carbon of preparation3VO4Nano particle shows that as lithium ion battery negative material charge and discharge capacity is 355 and 445 firstMAh/g, after 100 circulations, charge and discharge capacity is 419 and 420mAh/g, has shown higher specific capacity and has followed preferablyRing stability.
Embodiment 3
Take 1mmol vanadic anhydride, 3mmol lithium carbonate and 5mmol hexamethylenetetramine to beaker, add appropriateDistilled water stirs, and is transferred in hydro-thermal axe and reacts 140 degree 24 hours, and reaction gained solution is transferred in beaker and is added0.05mmol citric acid, fully stirs post-drying. Oven dry product is positioned in crucible, and crucible is moved into high temperature process furnancesIn, at 600 DEG C, under condition of nitrogen gas, to calcine 5 hours, the naturally cooling carbon that can obtain is coated Li3VO4Sample. Result shows, with instituteThe coated Li of carbon of preparation3VO4Nano particle shows that as lithium ion battery negative material charge and discharge capacity is 494 and 620 firstMAh/g, after 100 circulations, charge and discharge capacity is 496 and 498mAh/g, has shown higher specific capacity and excellent followingRing stability.
Claims (1)
1. the coated Li of carbon3VO4Lithium ion battery negative material, is characterized in that: this negative material be with vanadic anhydride,Lithium carbonate, hexamethylenetetramine and citric acid are basic material, the coated Li of carbon making3VO4Lithium ion battery negative material, shouldThe particle diameter of negative material is 90-120nm, in XRD collection of illustrative plates, is positioned at 16.3o、21.6o、22.9o、24.4o、28.2o、32.8o、36.3o、37.6o、49.8o、58.7o、66.2oWith 70.9oThe diffraction maximum at place corresponds respectively to rhombic system Li3VO4XRD cardSheet JCPDS, (100), (110) of No.38-1247, (011), (101), (111), (200), (002), (201), (202),(320), (203) and (322) crystal face;
Its concrete preparation method is to be raw material by 1mmol vanadic anhydride, 3mmol lithium carbonate and 5mmol hexamethylenetetramine, logicalCross hydro-thermal reaction and obtain middle phase solution, in the middle of then 0.05mmol citric acid being joined, in phase solution, mix, dryObtain solid product, this solid product is made after high-temperature atmosphere sintering to the coated Li of carbon3VO4Lithium ion battery negative material;Described hydrothermal temperature is 120 ~ 180 DEG C, and the reaction time is 12 ~ 48 hours; Described high-temperature atmosphere is nitrogen, sintering temperatureDegree is 500 ~ 600 DEG C, and sintering time 2 ~ 10 hours can make the coated Li of carbon3VO4Lithium ion battery negative material.
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| CN104852054A (en) * | 2015-04-13 | 2015-08-19 | 三峡大学 | N-doped carbon-coated Li3VO4 lithium ion battery composite anode material and preparation method |
| CN104868119A (en) * | 2015-04-16 | 2015-08-26 | 三峡大学 | Binder-free Li3VO4/C lithium ion battery cathode material and preparation method thereof |
| CN107039637A (en) * | 2016-02-03 | 2017-08-11 | 三峡大学 | A kind of high-performance negative material Li3VO4/ C preparation method and the application on sodium-ion battery |
| CN105552358A (en) * | 2016-02-03 | 2016-05-04 | 三峡大学 | Preparation method of chromium-doped Li<3>VO<4>/C anode material for lithium-ion battery |
| CN105742591A (en) * | 2016-03-02 | 2016-07-06 | 三峡大学 | Carbon coated Na3VO4 composite anode material and preparation method and application thereof |
| CN105529450A (en) * | 2016-03-02 | 2016-04-27 | 合肥国轩高科动力能源有限公司 | Preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability |
| CN105958029B (en) * | 2016-06-24 | 2018-06-05 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of composite cathode material of lithium ion battery lithium vanadate/carbon nanotubes/carbon |
| CN107845781B (en) * | 2016-09-19 | 2022-01-18 | 微宏动力***（湖州）有限公司 | Negative electrode active material for lithium ion secondary battery, method for producing same, and lithium ion secondary battery |
| CN106356510B (en) * | 2016-10-13 | 2019-06-04 | 中南大学 | A kind of ion cathode material lithium FeVO4The preparation method of/C |
| CN106941188B (en) * | 2017-05-03 | 2019-01-29 | 厦门大学 | One kind can charge and discharge aluminium ion battery and its preparation process |
| CN107293722B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | self-supporting NaVPO4F/C composite lithium ion battery anode and preparation method thereof |
| CN107492656B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | Self-supporting NaVPO4F/C sodium ion composite anode and preparation method thereof |
| CN107482181B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | Composite lithium ion battery anode material Li3V2(PO4)3/C and preparation method thereof |
| CN108666541B (en) * | 2018-04-16 | 2021-07-16 | 华南理工大学 | Sol-gel method for preparing carbon-coated VOMoO4Method for preparing lithium ion battery cathode material |
| CN112018373A (en) * | 2020-08-05 | 2020-12-01 | 嵊州市森拓新材料有限公司 | Carbon-coated Li with shell-core structure3VO4Lithium ion battery cathode material and preparation method thereof |
| CN112281258B (en) * | 2020-10-20 | 2022-10-04 | 三峡大学 | Li 3 VO 4 Negative electrode material of/C fiber lithium ion battery and preparation method |
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| CN103474641A (en) * | 2013-09-25 | 2013-12-25 | 三峡大学 | Lithium ion battery anode material Li3VO4 and preparation method thereof |
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