CN105870446A - Preparation method of modified graphene lithium ion battery anode material - Google Patents
Preparation method of modified graphene lithium ion battery anode material Download PDFInfo
- Publication number
- CN105870446A CN105870446A CN201610357730.6A CN201610357730A CN105870446A CN 105870446 A CN105870446 A CN 105870446A CN 201610357730 A CN201610357730 A CN 201610357730A CN 105870446 A CN105870446 A CN 105870446A
- Authority
- CN
- China
- Prior art keywords
- modified graphene
- lithium ion
- preparation
- ion battery
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- H01M4/58—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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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 preparation method of a modified graphene lithium ion battery anode material. The method comprises the steps that graphene, polyethyleneimine, polyvinyl alcohol and ethyl acetate are added to ethanol water, heating refluxing is conducted, filtering is conducted, and a solid mixture is obtained; vacuum solvent removing is conducted on the solid mixture, and modified graphene is obtained; modified graphene, butyl titanate, ammonium molybdate and polyethylene glycol are added into a reaction kettle, discharging is conducted after heating reacting is conducted, and an intermediate material is obtained; finally, the intermediate material is soaked with deionized water, filtering, drying and grinding are conducted, and the anode material is obtained. According to the anode material obtained through the preparation method, the initial capacity of the material is improved, and meanwhile the use stability is improved.
Description
Technical field
The invention belongs to lithium ion battery electrode material preparing technical field, be specifically related to the preparation method of a kind of modified graphene lithium ion battery negative material.
Background technology
Lithium ion battery is a kind of secondary cell (rechargeable battery), and it relies primarily on lithium ion and moves work between a positive electrode and a negative electrode.In charge and discharge process, Li+ comes and goes between two electrodes and embeds and deintercalation: during charging, and Li+, from positive pole deintercalation, embeds negative pole through electrolyte, and negative pole is in rich lithium state；During electric discharge the most contrary.Battery typically uses the material containing elemental lithium as electrode, is the representative of modern high performance battery.
Lithium ion battery refers to using two kinds of different lithium intercalation compound secondary cell systems as anode and negative pole that can reversibly embed and deviate from lithium ion.During charging, lithium ion, from positive pole deintercalation, by electrolyte and barrier film, is embedded in negative pole；During electric discharge then on the contrary, lithium ion, from negative pole deintercalation, by electrolyte and barrier film, is embedded in positive pole.The negative pole of lithium ion battery is to be mixed and made into pasty state adhesive uniform application in Copper Foil both sides by negative electrode active material, binding agent and additive, and drying, rolling form.Graphite, due to the advantage such as possess that electronic conductivity is high, lithium ion diffusion coefficient big, layer structure change in volume before and after embedding lithium lithium capacity little, embedding is high and intercalation potential is low, becomes the commercial Li-ion battery negative material of current main flow.Commercial Li-ion batteries mainly uses material with carbon element as negative electrode active material at present.But due to by theoretical specific capacity (
372mAh/g) restriction, the specific capacity of carbon negative pole material is difficult to improve further, it is therefore desirable to develops a kind of new negative material and promotes its specific capacity further, further expands application.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of modified graphene lithium ion battery negative material to overcome above the deficiencies in the prior art, promote the specific capacity of negative material.
Technical scheme is as follows:
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 10-20 part in parts by weight, polymine 5-10 part, polyvinyl alcohol 2-5 part, ethyl acetate 5-10 part joins in 80-100 part ethanol water, is heated to reflux 20-30 minute, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, obtains modified graphene；
Step 3, by modified graphene 10-20 part in parts by weight, butyl titanate 2-3 part, ammonium molybdate 1-4 part, Polyethylene Glycol 1-3 part joins in reactor, reacting by heating 20-30 minute, and discharging obtains intermediate material；
Step 4, uses deionized water to soak 3-5 hour by intermediate material, and filtering drying also grinds, and obtains negative material.
The preparation method of described modified graphene lithium ion battery negative material, in step one, the concentration of ethanol water is 70g
/100ml。
The preparation method of described modified graphene lithium ion battery negative material, in step 2, the vacuum of vacuum desolvation agent is 0.02-0.04MPa.
The preparation method of described modified graphene lithium ion battery negative material, in step 3, the heating-up temperature of reacting by heating is 80-90 DEG C.
The preparation method of described modified graphene lithium ion battery negative material, dries temperature and is 105-110 DEG C in step 4.
The preparation method of described modified graphene lithium ion battery negative material, is ground to particle diameter 400-600 micron in step 4.
The initial capacity of the modified graphene lithium ion battery negative material that the present invention provides has reached 156 more than mA/g, and the dump energy after 500 circulations is still more than 95%, hence it is evident that be better than existing Related product.
Detailed description of the invention:
Embodiment 1
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 10 parts in parts by weight, polymine 5 parts, polyvinyl alcohol 2 parts, ethyl acetate 5 parts joins in the ethanol water that 80 parts of concentration is 70g/100ml, is heated to reflux 20 minutes, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, and vacuum is 0.02MPa, obtains modified graphene；
Step 3, by modified graphene 10 parts in parts by weight, butyl titanate 2 parts, ammonium molybdate 1 part, Polyethylene Glycol 1 part joins in reactor, and under the conditions of 80 DEG C, reacting by heating 20 minutes, discharging, obtain intermediate material；
Step 4, uses deionized water to soak 3 hours by intermediate material, and filtering drying also grinds, and obtains negative material, and wherein drying temperature is 105 DEG C, is ground to particle diameter 400-600 micron.
Embodiment 2
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 12 parts in parts by weight, polymine 6 parts, polyvinyl alcohol 3 parts, ethyl acetate 7 parts joins in the ethanol water that 80 parts of concentration is 70g/100ml, is heated to reflux 25 minutes, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, and vacuum is 0.03MPa, obtains modified graphene；
Step 3, by modified graphene 15 parts in parts by weight, butyl titanate 2 parts, ammonium molybdate 3 parts, Polyethylene Glycol 1 part joins in reactor, and under the conditions of 85 DEG C, reacting by heating 23 minutes, discharging, obtain intermediate material；
Step 4, uses deionized water to soak 4 hours by intermediate material, and filtering drying also grinds, and obtains negative material, and wherein drying temperature is 105 DEG C, is ground to particle diameter 400-600 micron.
Embodiment 3
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 16 parts in parts by weight, polymine 7 parts, polyvinyl alcohol 4 parts, ethyl acetate 8 parts joins in the ethanol water that 90 parts of concentration is 70g/100ml, is heated to reflux 25 minutes, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, and vacuum is 0.03MPa, obtains modified graphene；
Step 3, by modified graphene 16 parts in parts by weight, butyl titanate 3 parts, ammonium molybdate 3 parts, Polyethylene Glycol 2 parts joins in reactor, and under the conditions of 90 DEG C, reacting by heating 28 minutes, discharging, obtain intermediate material；
Step 4, uses deionized water to soak 4 hours by intermediate material, and filtering drying also grinds, and obtains negative material, and wherein drying temperature is 100 DEG C, is ground to particle diameter 400-600 micron.
Embodiment 4
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 20 parts in parts by weight, polymine 10 parts, polyvinyl alcohol 5 parts, ethyl acetate 10 parts joins in the ethanol water that 100 parts of concentration is 70g/100ml, is heated to reflux 30 minutes, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, and vacuum is 0.04MPa, obtains modified graphene；
Step 3, by modified graphene 20 parts in parts by weight, butyl titanate 3 parts, ammonium molybdate 4 parts, Polyethylene Glycol 3 parts joins in reactor, and under the conditions of 90 DEG C, reacting by heating 30 minutes, discharging, obtain intermediate material；
Step 4, uses deionized water to soak 5 hours by intermediate material, and filtering drying also grinds, and obtains negative material, and wherein drying temperature is 110 DEG C, is ground to particle diameter 400-600 micron.
Reference examples
The preparation method of a kind of modified graphene lithium ion battery negative material, comprises the following steps:
Step one, by Graphene 16 parts in parts by weight, polymine 7 parts, polyvinyl alcohol 4 parts, 8 parts of mix homogeneously of ethyl acetate, obtains solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, and vacuum is 0.03MPa, obtains modified graphene；
Step 3, by modified graphene 16 parts in parts by weight, butyl titanate 3 parts, ammonium molybdate 3 parts, Polyethylene Glycol 2 parts joins in reactor, and under the conditions of 90 DEG C, reacting by heating 28 minutes, discharging, obtain intermediate material；
Step 4, uses deionized water to soak 4 hours by intermediate material, and filtering drying also grinds, and obtains negative material, and wherein drying temperature is 100 DEG C, is ground to particle diameter 400-600 micron.
The negative material preparing above example and reference examples carries out performance test, and result is as follows:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Reference examples |
| Initial capacity mA/g | 156 | 162 | 166 | 162 | 116 |
| Surplus % after 500 circulations | 95% | 95% | 96% | 96% | 87% |
As can be seen from the above results, the initial capacity of the modified graphene lithium ion battery negative material that the present invention provides has reached 156 more than mA/g, and the dump energy after 500 circulations is still more than 95%.Reference examples is the test carried out on the basis of embodiment 3, in preparation process one, wherein do not carry out ethanol water be heated to reflux, result causes final material initial capacity to decline substantially, after 500 circulations, surplus declines serious simultaneously, it can be seen that, in the preparation method that the present invention provides, the step of alcohol reflux is utilized to have important castering action for the performance of material.
Claims (6)
1. the preparation method of a modified graphene lithium ion battery negative material, it is characterised in that comprise the following steps:
Step one, by Graphene 10-20 part in parts by weight, polymine 5-10 part, polyvinyl alcohol 2-5 part, ethyl acetate 5-10 part joins in 80-100 part ethanol water, is heated to reflux 20-30 minute, is filtrated to get solid mixture；
Step 2, carries out vacuum desolvation agent by solid mixture, obtains modified graphene；
Step 3, by modified graphene 10-20 part in parts by weight, butyl titanate 2-3 part, ammonium molybdate 1-4 part, Polyethylene Glycol 1-3 part joins in reactor, reacting by heating 20-30 minute, and discharging obtains intermediate material；
Step 4, uses deionized water to soak 3-5 hour by intermediate material, and filtering drying also grinds, and obtains negative material.
The preparation method of modified graphene lithium ion battery negative material the most according to claim 1, it is characterised in that in step one, the concentration of ethanol water is 70g/100ml.
The preparation method of modified graphene lithium ion battery negative material the most according to claim 1, it is characterised in that in step 2, the vacuum of vacuum desolvation agent is 0.02-0.04MPa.
The preparation method of modified graphene lithium ion battery negative material the most according to claim 1, it is characterised in that in step 3, the heating-up temperature of reacting by heating is 80-90 DEG C.
The preparation method of modified graphene lithium ion battery negative material the most according to claim 1, it is characterised in that dry temperature in step 4 and be 105-110 DEG C.
The preparation method of modified graphene lithium ion battery negative material the most according to claim 1, it is characterised in that be ground to particle diameter 400-600 micron in step 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610357730.6A CN105870446A (en) | 2016-05-26 | 2016-05-26 | Preparation method of modified graphene lithium ion battery anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610357730.6A CN105870446A (en) | 2016-05-26 | 2016-05-26 | Preparation method of modified graphene lithium ion battery anode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105870446A true CN105870446A (en) | 2016-08-17 |
Family
ID=56641238
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610357730.6A Pending CN105870446A (en) | 2016-05-26 | 2016-05-26 | Preparation method of modified graphene lithium ion battery anode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105870446A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102569761A (en) * | 2010-12-08 | 2012-07-11 | 中国科学院金属研究所 | Titanium dioxide/graphene nanocomposite material and preparation method and application thereof |
| CN102923693A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Surface modification treatment method for graphene |
| CN103332678A (en) * | 2013-05-24 | 2013-10-02 | 东莞上海大学纳米技术研究院 | Preparation methods of graphene and graphene-oxide compound |
| CN103864066A (en) * | 2014-03-14 | 2014-06-18 | 嵇天浩 | Method for preparing graphene, MoS2 or WS2 microspheres |
-
2016
- 2016-05-26 CN CN201610357730.6A patent/CN105870446A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102569761A (en) * | 2010-12-08 | 2012-07-11 | 中国科学院金属研究所 | Titanium dioxide/graphene nanocomposite material and preparation method and application thereof |
| CN102923693A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Surface modification treatment method for graphene |
| CN103332678A (en) * | 2013-05-24 | 2013-10-02 | 东莞上海大学纳米技术研究院 | Preparation methods of graphene and graphene-oxide compound |
| CN103864066A (en) * | 2014-03-14 | 2014-06-18 | 嵇天浩 | Method for preparing graphene, MoS2 or WS2 microspheres |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2020064866A (en) | Aqueous slurry for battery electrode | |
| CN103117414B (en) | A kind of negative pole lithium titanate battery electrolyte, lithium ion battery and preparation method thereof | |
| WO2016201940A1 (en) | Preparation method for carbon/graphite composite anode material | |
| CN105742641A (en) | Conductive coating and lithium-ion battery employing same | |
| WO2017024720A1 (en) | Preparation method for high capacity lithium-ion battery negative electrode material | |
| CN105870452A (en) | Anode material, lithium ion battery with anode material and preparation method | |
| CN101859886A (en) | Lithium ion battery anode material and preparation method thereof | |
| CN110690437B (en) | Sodium ion battery negative electrode sodium supplement additive, sodium ion battery negative electrode piece and sodium ion battery | |
| CN103117412B (en) | Lithium ion battery and chemical synthesizing method thereof | |
| CN105742695B (en) | A kind of lithium ion battery and preparation method thereof | |
| CN104577120A (en) | Preparation method of lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material | |
| CN102664247B (en) | Method for preparing LiFePO4/SiC lithium battery positive plate by microwave heating | |
| CN102610790A (en) | Lithium ion secondary battery and anode plate of lithium ion secondary battery | |
| CN103107309B (en) | A kind of lithium ion cell positive and preparation method thereof | |
| CN114380282B (en) | Modified sodium vanadium phosphate positive electrode material and preparation method and application thereof | |
| CN116845214A (en) | Sodium supplementing additive and carbon co-coated composite sodium iron phosphate positive electrode material and preparation method thereof | |
| KR101635752B1 (en) | Electrode binder composition for controlling the drying rate, the electrode and lithium secondary cell comprising the same | |
| CN104766961B (en) | Preparation method of low-specific-surface-area carbon/carbon composite negative electrode material of sodium ion battery | |
| WO2018023321A1 (en) | Preparation method for positive electrode sheet containing lithium-ion conductive polymer coating | |
| CN114335460B (en) | Quick-filling graphite composite material and preparation method thereof | |
| CN109921023A (en) | Lithium ion battery preparation and the application method for being cross-linked in situ three-dimensional netted binder | |
| CN105870446A (en) | Preparation method of modified graphene lithium ion battery anode material | |
| CN107240713A (en) | A kind of method for improving battery charge efficiency | |
| CN109309228B (en) | Positive electrode active material, preparation method, positive electrode and high-specific-energy power battery | |
| CN110571409B (en) | Preparation method of anode material, anode material and lithium battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160817 |
|
| RJ01 | Rejection of invention patent application after publication |