CN104868119A - Binder-free Li3VO4/C lithium ion battery cathode material and preparation method thereof - Google Patents
Binder-free Li3VO4/C lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN104868119A CN104868119A CN201510179328.9A CN201510179328A CN104868119A CN 104868119 A CN104868119 A CN 104868119A CN 201510179328 A CN201510179328 A CN 201510179328A CN 104868119 A CN104868119 A CN 104868119A
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- ion battery
- lithium ion
- li3vo4
- liquid
- cathode material
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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
- H01M10/05—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
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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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a binder-free lithium ion battery cathode material. A structure of the cathode material is Li3VO4/C/Ni. A preparation method of the cathode material comprises the steps of weighing ammonium metavanadate, lithium carbonate and hexamethylene tetramine at a mole ratio of 2:3:5, placing ammonium metavanadate, lithium carbonate and hexamethylene tetramine in a beaker, adding an appropriate amount of deionized water, performing stirring to obtain a uniform solution, placing the uniform solution in a hydrothermal reaction kettle, performing a reaction for 4-20h at 90-180 DEG C to obtain precursor liquid, adding an appropriate amount of citric acid to the precursor liquid, performing uniform stirring, immersing a foam nickel matrix into the liquid, taking the nickel matrix out after standing for some time, performing drying at 50-70 DEG C, and sintering a drying product for 2-10h at 400-600 DEG C under a nitrogen condition to obtain an Li3VO4/C/Ni composite electrode. An active substance in the battery cathode material is Li3VO4/C which is directly deposited on the surface of foam nickel and well contacted with the foam nickel; Li3VO4/C in a prepared sample is granular; the average size is about 200nm; and the prepared sample can directly serve as a lithium ion battery cathode without a binder.
Description
Technical field
The present invention relates to a kind of preparation technology of Novel cathode material for lithium ion battery, particularly a kind of Li
3vO
4/ C composite binder free technology for preparing electrode, belongs to field of electrochemical power source.
technical background:
Lithium ion battery is widely used in field of portable electronic apparatus because of its superior performance.But, due to its limitation in fail safe, energy density, cycle performance etc., limit its application in fields such as electric automobile, hybrid vehicle, intelligent grids.At present, commercial li-ion cell positive material system is relatively abundant, but negative material is still confined to material with carbon element, and its theoretical capacity is lower, and the security hidden trouble that under there is electronegative potential, Li dendrite is separated out.Therefore, research and development have safety, high-energy-density, long circulating performance new type lithium ion negative material significant.Li
3vO
4as a kind of Novel anode material, there is more high-volume and capacity ratio and better security performance, compared to Li compared to commercial graphite negative electrodes material
4ti
5o
12negative material has higher specific capacity, lower charge and discharge voltage, and current commercial positive electrode coupling is good, has broad application prospects in lithium ion battery.Restriction Li
3vO
4in lithium ion battery, the main cause of practical application is that its electronic conductivity is lower, and this can cause, and its charge and discharge voltage polarizing is comparatively large, high rate performance is undesirable.Existing research is mainly through by Li
3vO
4with carbon compound to improve its conductivity, thus promote its chemical property.At present, conventional lithium ion battery negative pole preparation technology is that be coated in after stirring on Copper Foil, technology for preparing electrode is more loaded down with trivial details by electrode material, binding agent, conductive agent mixing, and Cathode uniformity is difficult to control and is difficult to ensure the contact of active material and conducting base.In addition, the binding agent introduced in electrode production process itself does not store up lithium activity, and conductive agent mostly is amorphous carbon material, and theoretical capacity is also lower, and this will cause certain capacitance loss.Compare traditional technology for preparing electrode, directly deposition growing active material thus prepare binder free electrode on foam metal, technology for preparing electrode can not only be simplified, the high-specific surface area of foam metal can also be utilized, good conductivity and structural stability improve the electrochemical reaction dynamics of active material, the structural stability of enhanced activity material in cyclic process, thus promote its chemical property, these research and development for high performance lithium ion battery have great importance.At present, about binder free Li
3vO
4there is not been reported in the research of/C electrode.
Based on above background, a kind of Li of invention
3vO
4/ C/Ni binder free lithium ion battery negative.Take nickel foam as conducting base, by adsorption Li
3vO
4presoma and the mixed uniformly liquid of carbon source, then in-situ sintering prepares Li
3vO
4/ C contacts good Li with Ni substrate
3vO
4/ C/Ni electrode.With prepared Li
3vO
4/ C/Ni shows good cyclical stability as lithium ion battery negative.
goal of the invention:
Object of the present invention is exactly with ammonium metavanadate, lithium carbonate, hexamethylenetetramine for reaction raw materials, take citric acid as carbon source, with metal foam nickel for conducting base, prepares binder free Li by hydro-thermal reaction, presoma absorption, in-situ sintering
3vO
4/ C/Ni negative pole.Its principle is exactly first utilize hydro-thermal reaction to prepare precursor solution, introduces citric acid as carbon source, immerses in transparency liquid subsequently by nickel foam substrate, dry and obtain Li eventually through solid phase reaction
3vO
4/ C/Ni electrode.
Li involved in the present invention
3vO
4/ C/Ni electrode synthesis material is ammonium metavanadate, lithium carbonate, hexamethylenetetramine, citric acid, nickel foam.In material preparation process, first by ammonium metavanadate, lithium carbonate and hexamethylenetetramine in molar ratio 2:3:5 take, be positioned in beaker and add appropriate amount of deionized water and stir, be then transferred in hydrothermal reaction kettle and react 4 ~ 20 hours (more preferably reacting 6h at 150 DEG C) at 90 ~ 180 DEG C.The solution be obtained by reacting to be transferred in beaker and to add a certain amount of citric acid, after abundant stirring, nickel foam substrate is immersed, take out after leaving standstill a period of time and dry, finally be heated to 400 ~ 600 DEG C of sintering, 2 ~ 10 hours (more preferably sintering 5h at 500 DEG C) under a nitrogen atmosphere, cooling can obtain Li naturally
3vO
4/ C/Ni electrode.
Li involved in the present invention
3vO
4/ C/Ni electrode and preparation method have following distinguishing feature:
(1) electrode preparation method is simple, is easy to operation;
(2) in electrode, active material is Li
3vO
4/ C, is deposited directly to nickel foam surface, contacts well with nickel foam;
(3) Li in prepared sample
3vO
4/ C is graininess, average-size about 200 nm.
(4) prepared sample directly can be used as lithium ion battery negative, without the need to binding agent.
accompanying drawing illustrates:
The Raman (a) of sample prepared by Fig. 1 embodiment 1 and XRD (b) collection of illustrative plates.
The SEM figure of sample prepared by Fig. 2 embodiment 1.
(a) of sample prepared by Fig. 3 embodiment 1 be charge and discharge curve and (b) cycle performance figure first.
(a) of sample prepared by Fig. 4 embodiment 2 be charge and discharge curve and (b) cycle performance figure first.
(a) of sample prepared by Fig. 5 embodiment 3 be charge and discharge curve and (b) cycle performance figure first.
embodiment:
embodiment 1
Take 2 mmol ammonium metavanadates, 3 mmol lithium carbonates and 5 mmol hexamethylenetetramines in beaker, add appropriate amount of deionized water and fully stir and obtain clear solution, be transferred to by solution in hydro-thermal axe, under 140 DEG C of conditions, reaction obtains precursor liquid in 6 hours.Precursor liquid to be transferred in beaker and to add 0.05 g citric acid, after fully stirring, nickel foam substrate being immersed, leaving standstill after 5 hours and take out and 60 DEG C of oven dry in an oven.Be positioned in crucible by the nickel foam of oven dry, move in high temperature process furnances, at 500 DEG C, sinter 5 hours under condition of nitrogen gas, cooling obtains Li naturally
3vO
4/ C/Ni sample.Prepared sample through Raman analysis, as shown in Fig. 1 (a), Raman peaks and Li
3vO
4(★) corresponding with C (△).Through XRD atlas analysis, as shown in Fig. 1 (b), with Li
3vO
4(★) corresponding with the diffraction maximum of nickel foam (zero).Prepared Li
3vO
4/ C/Ni sample characterizes through SEM, as seen from Figure 3, and Li
3vO
4/ C uniform deposition is surperficial in nickel foam, in graininess, and particle mean size about 200 nm.Embodiment 1 gained sample is made button cell as follows: by obtained Li
3vO
4/ C/Ni sample is cut into the disk that diameter is 14 mm, vacuumize 12 hours at 120 DEG C.Be to electrode with metal lithium sheet, Celgard film is barrier film, is dissolved with LiPF
6eC+DMC+DEC (volume ratio the is 1:1:1) solution of (1 mol/L) is electrolyte, is assembled into CR2025 type battery in the glove box of argon shield.Battery pack installs rear standing 8h, then carries out constant current charge-discharge test with CT2001A battery test system, and test voltage is 3 ~ 0.02 V.Fig. 3 shows, the Li prepared by embodiment 1
3vO
4/ C/Ni electrode first charge and discharge capacity is respectively 653 and 859 mAh/g, and after 100 circulations, charge and discharge capacity is 511 and 513 mAh/g, shows higher specific capacity and excellent stable circulation performance.
embodiment 2
Take 2 mmol ammonium metavanadates, 3 mmol lithium carbonates and 5 mmol hexamethylenetetramines in beaker, add appropriate amount of deionized water and fully stir and obtain clear solution, be transferred to by solution in hydro-thermal axe, under 140 DEG C of conditions, reaction obtains precursor liquid in 6 hours.Precursor liquid to be transferred in beaker and to add 0.05 g citric acid, after fully stirring, nickel foam substrate being immersed, leaving standstill after 5 hours and take out and 60 DEG C of oven dry in an oven.Be positioned in crucible by the nickel foam of oven dry, move in high temperature process furnances, at 400 DEG C, sinter 5 hours under condition of nitrogen gas, cooling obtains Li naturally
3vO
4/ C/Ni sample.With prepared sample for negative pole, will button cell be prepared into by step in embodiment 1 and its chemical property will be analyzed.As shown in Figure 4, the Li prepared by embodiment 2
3vO
4/ C/Ni electrode first charge and discharge capacity is respectively 468 and 498 mAh/g, and after 100 circulations, charge and discharge capacity is 376 mAh/g.
embodiment 3
Take 2 mmol ammonium metavanadates, 3 mmol lithium carbonates and 5 mmol hexamethylenetetramines in beaker, add appropriate amount of deionized water and fully stir and obtain clear solution, be transferred to by solution in hydro-thermal axe, under 140 DEG C of conditions, reaction obtains precursor liquid in 6 hours.Precursor liquid to be transferred in beaker and to add 0.05 g citric acid, after fully stirring, nickel foam substrate being immersed, leaving standstill after 5 hours and take out and 60 DEG C of oven dry in an oven.Be positioned in crucible by the nickel foam of oven dry, move in high temperature process furnances, at 600 DEG C, sinter 5 hours under condition of nitrogen gas, cooling obtains Li naturally
3vO
4/ C/Ni sample.With prepared sample for negative pole, be prepared into button cell by step in embodiment 1 and its chemical property is analyzed.As shown in Figure 5, the Li prepared by embodiment 3
3vO
4/ C/Ni electrode first charge and discharge capacity is respectively 528 and 712 mAh/g, and after 100 circulations, charge and discharge capacity is respectively 428 and 429 mAh/g.
Claims (2)
1. a binder free lithium ion battery negative material, is characterized in that, the structure of this negative material is Li
3vO
4/ C/Ni;
The concrete preparation method of described lithium ion battery negative material is:
(1) by analyzing the chemical raw material ammonium metavanadate of pure (99.9%), lithium carbonate, hexamethylenetetramine take for 2:3:5 in molar ratio, is positioned in beaker to add appropriate amount of deionized water and stir, and obtains homogeneous solution;
(2) liquid that step (1) obtains is positioned in hydrothermal reaction kettle and reacts 4 ~ 20 hours at 90 ~ 180 DEG C, obtain precursor liquid;
(3) add appropriate citric acid in the precursor liquid obtained to step (2), stir, subsequently nickel foam substrate is immersed in liquid, take out after leaving standstill a period of time, and 50 ~ 70 DEG C of oven dry;
(4) product step (3) obtained is at 400 ~ 600 DEG C, and under condition of nitrogen gas, namely sintering obtains Li in 2 ~ 10 hours
3vO
4/ C/Ni combination electrode.
2. a binder free lithium ion battery negative material, is characterized in that, the structure of this negative material is Li
3vO
4/ C/Ni;
The concrete preparation method of described lithium ion battery negative material is:
(1) by analyzing the chemical raw material ammonium metavanadate of pure (99.9%), lithium carbonate, hexamethylenetetramine take for 2:3:5 in molar ratio, is positioned in beaker to add appropriate amount of deionized water and stir, and obtains homogeneous solution;
(2) liquid that step (1) obtains is positioned in hydrothermal reaction kettle and reacts 6 hours at 140 DEG C, obtain precursor liquid;
(3) add appropriate citric acid in the precursor liquid obtained to step (2), stir, subsequently nickel foam substrate is immersed in liquid, take out after leaving standstill a period of time, and 60 DEG C of oven dry;
(4) product step (3) obtained is at 500 DEG C, and under condition of nitrogen gas, namely sintering obtains Li in 5 hours
3vO
4/ C/Ni combination electrode.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105390681A (en) * | 2015-12-03 | 2016-03-09 | 三峡大学 | Binder-free lithium ion battery negative electrode material and preparation method therefor |
| 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 |
| CN106941188A (en) * | 2017-05-03 | 2017-07-11 | 厦门大学 | One kind can discharge and recharge aluminium ion battery and its preparation technology |
| 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 |
| CN107293723A (en) * | 2017-07-10 | 2017-10-24 | 三峡大学 | A kind of binder free Na3V2(PO4)3/ C composite lithium ion battery anodes and preparation method thereof |
| CN107293722A (en) * | 2017-07-10 | 2017-10-24 | 三峡大学 | A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof |
| CN107317017A (en) * | 2017-07-10 | 2017-11-03 | 三峡大学 | A kind of binder free Na3V2(PO4)3/ C is combined sodium-ion battery positive pole and preparation method thereof |
| CN107492656A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of self-supporting NaVPO4F/C sodium ion anode composites and preparation method thereof |
| CN107492634A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof |
| CN109860603A (en) * | 2019-01-21 | 2019-06-07 | 珠海光宇电池有限公司 | Lithium battery pole slice and preparation method thereof and lithium battery |
| CN111082027A (en) * | 2019-12-31 | 2020-04-28 | 三峡大学 | Preparation method of biomass carbon lithium ion battery cathode material |
| CN112281258A (en) * | 2020-10-20 | 2021-01-29 | 三峡大学 | Li3VO4Negative electrode material of/C fiber lithium ion battery and preparation method |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105390681A (en) * | 2015-12-03 | 2016-03-09 | 三峡大学 | Binder-free lithium ion battery negative electrode material and preparation method therefor |
| 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 |
| 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 |
| CN106941188A (en) * | 2017-05-03 | 2017-07-11 | 厦门大学 | One kind can discharge and recharge aluminium ion battery and its preparation technology |
| CN107492634A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof |
| CN107293723B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | Binder-free Na3V2(PO4)3/C lithium ion battery composite anode and preparation method thereof |
| CN107317017A (en) * | 2017-07-10 | 2017-11-03 | 三峡大学 | A kind of binder free Na3V2(PO4)3/ C is combined sodium-ion battery positive pole and preparation method thereof |
| CN107492656A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of self-supporting NaVPO4F/C sodium ion anode composites and preparation method thereof |
| CN107293723A (en) * | 2017-07-10 | 2017-10-24 | 三峡大学 | A kind of binder free Na3V2(PO4)3/ C composite lithium ion battery anodes and preparation method thereof |
| CN107317017B (en) * | 2017-07-10 | 2020-06-02 | 三峡大学 | Binder-free Na3V2(PO4)3Positive electrode of/C composite sodium ion battery 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 |
| CN107293722A (en) * | 2017-07-10 | 2017-10-24 | 三峡大学 | A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof |
| CN107492634B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | binder-free Li3V2(PO4)3/C composite lithium ion battery anode and preparation method thereof |
| 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 |
| CN109860603A (en) * | 2019-01-21 | 2019-06-07 | 珠海光宇电池有限公司 | Lithium battery pole slice and preparation method thereof and lithium battery |
| CN111082027A (en) * | 2019-12-31 | 2020-04-28 | 三峡大学 | Preparation method of biomass carbon lithium ion battery cathode material |
| CN112281258A (en) * | 2020-10-20 | 2021-01-29 | 三峡大学 | Li3VO4Negative electrode material of/C fiber lithium ion battery and preparation method |
| 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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