CN106532046A - Lithium-doped graphite negative electrode material and preparation method thereof - Google Patents
Lithium-doped graphite negative electrode material and preparation method thereof Download PDFInfo
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- CN106532046A CN106532046A CN201510897572.9A CN201510897572A CN106532046A CN 106532046 A CN106532046 A CN 106532046A CN 201510897572 A CN201510897572 A CN 201510897572A CN 106532046 A CN106532046 A CN 106532046A
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- lithium
- graphite
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
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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 discloses a lithium-doped graphite negative electrode material and a preparation method thereof. The preparation method of the lithium-doped graphite negative electrode material comprises the following steps of (1) accurately weighing a certain mass of LiOH.H2O, adding the LiOH.H2O to 250ml of deionized water to prepare 1-100g/ml of lithium solution, adding a certain mass of graphite powder and stirring for 1h; (2) adding the evenly stirred mixed solution to a hydrothermal reaction kettle, controlling a system temperature to be 100-180 DEG C and carrying out hydrothermal reaction for 1-24h; (3) naturally cooling the product to a room temperature after reaction is completed, cleaning the product by using the deionized water and ethyl alcohol for 4 times separately, and then drying the product in a drying oven at 30-100 DEG C for 3-25h; and (4) putting the dried powder into a tube furnace, heating the powder to 300-800 DEG C at a speed of 10 DEG C/min and keeping the constant temperature for 1-24h. The discharge capacity of the prepared graphite negative electrode material can reach 359.5, the initial efficiency can reach 94.1% and the capacity retention ratio is 90.18% after 500 charge-discharge cycles at 1C.
Description
Technical field
The present invention relates to material and electrochemical field, specifically one kind mix lithium graphite cathode material and its preparation side
Method.
Background technology
With the development of science and technology, people put forward higher requirement to the performance of electrochmical power source (battery).
Such as:The development of integrated circuit technique makes electronic instrument small, portability, correspondingly requires that battery has body
The characteristics of product is little, lightweight, specific energy is high；Space exploration technology and national defence, the continuous of military equipment technology send out
Exhibition requires that battery has high-energy-density and long storage life；The reinforcement of environmental protection consciousness makes people to electric automobile
Development growing interest, and this battery should then have big specific energy and specific power.In numerous battery systems
In, clang battery is so that its operating voltage is high, big energy density and show one's talent the advantages of light weight, by countries in the world
Attention.
At present, graphite cathode material becomes the first-selected negative material of commercialization lithium battery due to its excellent performance,
Thus the research to graphite cathode does not stop always, high power capacity and high efficiency first are one of hot fields.
The content of the invention
It is an object of the invention to provide one kind mixes lithium graphite cathode material and preparation method thereof, it is above-mentioned to solve
Capacity and efficiency first is proposed in background technology；
For achieving the above object, the present invention provides following technical scheme：
One kind mixes lithium graphite cathode material and preparation method thereof, including：
Step one：The Li0H.H of certain mass is weighed accurately20 be added to 250ml deionized waters in be configured to
Certain density Li0H.H20 aqueous solution, adds a certain amount of graphite powder, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, control system temperature
100-180 DEG C, hydro-thermal reaction 1-24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
3-25h is dried at 30-100 DEG C in drying box afterwards.
Step 4：Dried powder is put in tube furnace to heat and is warmed up to 10 DEG C/min
300-800 DEG C, constant temperature 1-24h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
The Li0H.H2Li0H.H in 0 aqueous solution20 quality is 2-40g.
The graphite powder includes native graphite, natural spherical plumbago, natural flake graphite, Delanium,
MCMB is therein one or more.
The particle diameter (D50) of the graphite powder is between 1 μm -50 μm；
The quality of the graphite powder is between 100g-400g
The hydro-thermal reaction includes the one kind in conventional hydrothermal, microwave hydrothermal and homogeneous hydro-thermal.
The present invention principle be：
The present invention passes through doped lithium ion element in graphite so as to form composite, and doping elemental lithium is to be formed
The chemical constituent of SEI films, thus the graphite electrode of elements doped lithium is lost for forming SEI films in embedding lithium first
Irreversible capacity be effectively suppressed, so as to Reversible lithium insertion capacity increases, improve efficiency first.
The inventive method has novelty, easy to operation, and repeatable strong, low cost, to environment
Free of contamination feature.The cathode material of lithium ion battery prepared using the inventive method, with cyclical stability
By force, the characteristics of electric conductivity is strong.
Description of the drawings
Fig. 1 is the soft-package battery loop test curve of the embodiment of the present invention 6.
Fig. 2 is the scanning electron microscopic picture of the embodiment of the present invention 6.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground description, it is clear that described embodiment is only a part of embodiment of the invention, rather than the enforcement of whole
Example.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The every other embodiment for being obtained, belongs to the scope of protection of the invention.
Embodiment 1
Step one：The Li0H.H of 10g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 300 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 2
Step one：The Li0H.H of 15g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 20g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 300 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 3
Step one：The Li0H.H of 20g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 300 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 4
Step one：30g Li0H.H are weighed accurately20 be added to 250ml deionized waters in be configured to it is certain dense
The Li0H.H of degree20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 300 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 5
Step one：The Li0H.H of 40g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 300 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 6
Step one：The Li0H.H of 20g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 500 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 7
Step one：The Li0H.H of 20g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 700 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Embodiment 8
Step one：The Li0H.H of 20g is weighed accurately20 be added to 250ml deionized waters in be configured to it is certain
The Li0H.H of concentration20 aqueous solution, adds the Delanium of 200g, stirs 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, 100 DEG C of control system temperature,
Hydro-thermal reaction 24h；
Step 3：Reaction naturally cools to room temperature after terminating, respectively deionized water and ethanol purge 4 times
5h is dried in drying box 80 DEG C afterwards.
Step 4：Dried powder is put in tube furnace to heat 800 DEG C are warmed up to 10 DEG C/min,
Constant temperature 3h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in vacuum drying chamber
It is standby.
Half-cell method of testing used by of the invention is：Graphite sample, the N- containing 6～7% Kynoar
Methyl pyrrolidone and 2% conductive black are well mixed, and be applied on Copper Foil, the pole piece for coating is put into temperature
It is standby for being vacuum dried 4 hours in 110 DEG C of vacuum drying chambers.Simulated battery is assemblied in the German Blaw of applying argon gas
Carry out in grace glove box, electrolyte be 1M LiPF6+EC: DEC: DMC=1: 1: 1 (volume ratio), metal
Lithium piece is that, to electrode, electrochemical property test is carried out on U.S. ArbinBT2000 type cell testers, charge and discharge
Piezoelectric voltage scope is 0.005 to 1.0V, and charge-discharge velocity is 0.1C.Data are listed in Table 1, and comparative example is
The Delanium of undoped p elemental lithium.
Used by of the invention, full battery testing method is：The graphite of the embodiment of the present invention or comparative example makees negative pole, cobalt
Sour lithium makees positive pole, and 1M-LiPF6EC: DMC: EMC=1: 1: 1 (volume ratio) solution is made electrolyte assembling and helped
Battery, in 500 weeks capability retentions of 1C charge and discharges 90.18%, comparative example is undoped p lithium to testing example 6
The Delanium of element, as shown in Figure 1.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and
And without departing from the spirit or essential characteristics of the present invention, this can be realized in other specific forms
It is bright.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and is non-limiting
, the scope of the present invention is by claims rather than described above is limited, it is intended that will fall will in right
All changes in the implication and scope of the equivalency asked are included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment party
Formula only includes an independent technical scheme, and this narrating mode of specification is only ability for clarity
Field technique personnel should be using specification as an entirety, and the technical scheme in each embodiment can also appropriate group of Jing
Close, formed it will be appreciated by those skilled in the art that other embodiment.
Claims (6)
1. one kind mixes lithium graphite cathode material, it is characterised in that include：
Step one：The Li0H.H of certain mass is weighed accurately20 be added to 250ml deionized waters in be configured to the lithium solution of 1-100g/ml, add a certain amount of graphite powder, stir 1h；
Step 2：The mixed liquor for stirring is added in hydrothermal reaction kettle, control system temperature 100-180 DEG C, hydro-thermal reaction 1-24h；
Step 3：Reaction naturally cools to room temperature after terminating, and is dried 3-25h at 30-100 DEG C in drying box respectively after deionized water and ethanol purge 4 times；
Step 4：Dried powder is put in tube furnace to heat 300-800 DEG C is warmed up to 10 DEG C/min, constant temperature 1-24h.
Step 5：Naturally cool to room temperature and obtain final product negative material to be invented, be placed in standby in vacuum drying chamber.
2. one kind according to claim 1 mixes lithium graphite cathode material, it is characterised in that the Li0H.H2Li0H.H in 0 aqueous solution20 quality is 2-40g.
3. one kind according to claim 1 mixes lithium graphite cathode material, it is characterised in that the graphite powder includes native graphite, and natural spherical plumbago, natural flake graphite, Delanium, MCMB are therein one or more.
4. one kind according to claim 1 mixes lithium graphite cathode material and preparation method thereof, it is characterised in that the particle diameter of the graphite powder is between 1 μm -50 μm.
5. one kind according to claim 1 mixes lithium graphite cathode material, it is characterised in that the quality of the graphite powder is between 100g-400g.
6. one kind according to claim 1 mixes lithium graphite cathode material, it is characterised in that the hydro-thermal reaction includes the one kind in conventional hydrothermal (high-pressure digestion tank method), microwave hydrothermal and homogeneous hydro-thermal.
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| CN201510897572.9A CN106532046A (en) | 2015-12-08 | 2015-12-08 | Lithium-doped graphite negative electrode material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106785007A (en) * | 2017-03-27 | 2017-05-31 | 中天储能科技有限公司 | A kind of lithium ion battery of coulombic efficiency first high |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN109616637A (en) * | 2018-12-05 | 2019-04-12 | 中南大学 | A kind of lithium ion battery negative material of high coulomb efficiency and cycle life |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104393235A (en) * | 2014-04-21 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Lithium-salt-modified lithium ion battery anode material and preparation method thereof |
| CN104538630A (en) * | 2014-12-17 | 2015-04-22 | 李震祺 | Lithium ion battery negative material and preparation method thereof |
-
2015
- 2015-12-08 CN CN201510897572.9A patent/CN106532046A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104393235A (en) * | 2014-04-21 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Lithium-salt-modified lithium ion battery anode material and preparation method thereof |
| CN104538630A (en) * | 2014-12-17 | 2015-04-22 | 李震祺 | Lithium ion battery negative material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106785007A (en) * | 2017-03-27 | 2017-05-31 | 中天储能科技有限公司 | A kind of lithium ion battery of coulombic efficiency first high |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN109616637A (en) * | 2018-12-05 | 2019-04-12 | 中南大学 | A kind of lithium ion battery negative material of high coulomb efficiency and cycle life |
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Application publication date: 20170322 |