CN107482168A - Low temperature lithium battery anode and preparation method thereof - Google Patents
Low temperature lithium battery anode and preparation method thereof Download PDFInfo
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- CN107482168A CN107482168A CN201710600465.4A CN201710600465A CN107482168A CN 107482168 A CN107482168 A CN 107482168A CN 201710600465 A CN201710600465 A CN 201710600465A CN 107482168 A CN107482168 A CN 107482168A
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- 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
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- 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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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention provides a kind of low temperature lithium battery anode and preparation method thereof, including major ingredient, solvent and additive, major ingredient is LiFePO4 or ternary, solvent NMP, and additive includes PVDF, SP, KS 6 and multi-layer graphene；Multi-layer graphene accounts for the 2 7% of positive pole gross mass；Multi-layer graphene includes multilayer chip graphene and diamond, and diamond is located between adjacent two layers of multilayer chip graphene, and the carbon atom of diamond and multilayer chip graphene corresponds.The present invention adds new additive material in the positive pole of lithium battery, realize in the relatively low environment of temperature, the electronics and ion channel got through battery electrolyte low-temperature setting and blocked, increase the purpose of ion activity, so that battery can preferably work when low temperature, minimum to be worked in the environment of 40 DEG C, the moment for avoiding lithium battery from being opened in electronic product burns, the security that increase lithium ion works at low ambient temperatures.
Description
Technical field
The present invention relates to technical field of lithium batteries, more particularly, to a kind of low temperature lithium battery anode and preparation method thereof.
Background technology
Lithium ion battery:It is a kind of secondary cell (rechargeable battery), it relies primarily on lithium ion between a positive electrode and a negative electrode
Movement carrys out work.In charge and discharge process, Li+ comes and goes insertion and deintercalation between two electrodes:During charging, Li+ takes off from positive pole
It is embedding, negative pole is embedded in by electrolyte, negative pole is in rich lithium state；It is then opposite during electric discharge.The electrolyte according to used in lithium ion battery
The difference of material, lithium ion battery are divided into liquid lithium ionic cell and polymer Li-ion battery.Wherein, liquid lithium ionic cell
Refer to the secondary cell that Li+ inlaid schemes are positive and negative electrode.Positive pole uses lithium compound, and negative pole uses chemical combination between lithium-carbon-coating
Thing.The normal operating temperature range of lithium ion battery is -20 DEG C~60 DEG C, and the freezing point of lithium ion battery electrolyte solution is -40
DEG C, easily freezing, environment below freezing is there is a possibility that lithium battery burns in the moment that electronic product is opened, therefore, people from this area
Member tries to explore, and to develop a kind of new material to improve the operating temperature range of lithium ion battery, makes lithium-ion electric
Pond can in the environment of less than -20 DEG C normal work, the moment for avoiding lithium battery from being opened in electronic product burn, increase lithium ion
The security to work at low ambient temperatures.
The content of the invention
The present invention solves the technical problem of a kind of low temperature lithium battery anode and preparation method thereof is provided, new is added
Add agent material to add in the positive pole of lithium battery, realize in the relatively low environment of temperature, get through battery electrolyte low-temperature setting and block up
The electronics and ion channel of plug, increase the purpose of ion activity, so that battery can preferably work when low temperature, most
Low to be worked in the environment of -40 DEG C, the moment for avoiding lithium battery from being opened in electronic product burns, and increase lithium ion is in low temperature
The security to be worked under environment.
In order to solve the above technical problems, one aspect of the present invention is：A kind of low temperature lithium battery anode is provided
And preparation method thereof, including major ingredient, solvent and additive, the major ingredient are LiFePO4 or ternary, the solvent is NMP (N-
Methyl pyrrolidone), the additive include PVDF (Kynoar), SP (ultra-fine carbon dust), KS-6 (graphite agent) and
Multi-layer graphene；
The weight percentage of each component is as follows：The major ingredient is 40-46%, the NMP is 47-50%, the PVDF
For 2-3%, the SP be 1-2%, the KS-6 is 1-2% and the multi-layer graphene is 2-7%；
The multi-layer graphene includes multilayer chip graphene and diamond, and the diamond is located at multilayer chip graphene
Adjacent two layers between, the carbon atom of the diamond and described multilayer chip graphene corresponds；
The weight ratio of the multilayer chip graphene and the diamond is (4-6)：1；
The multilayer chip graphene is 6-8 lamellar graphenes, and every layer of thickness of the multilayer chip graphene is
0.3-0.7nm, the interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.1-0.5nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.7-1.6nm.
Further say, the weight ratio of the multilayer chip graphene and the diamond is 5：1；
The number of plies of the multilayer chip graphene is 8 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.5nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.3nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.9nm.
Further say, the preparation method of the multi-layer graphene, comprise the following steps：
Step 1: multilayer chip graphene is prepared using chemical deposition：With cathode-ray on silica substrate surface
One layer of nickel metal layer is deposited, the thickness of the nickel metal layer is 200-400nm；
Step 2: be passed through in the tube furnace of 950-1150 DEG C of temperature methane, hydrogen and ammonia composition gaseous mixture and
Common graphite powder, room temperature is cooled within 100ms, obtains multilayer chip graphene, the layer of multilayer chip graphene described herein
Number is 3-12 layers；
Step 3: more than 100,000 grades under cleanliness factor environment, by being peeled off after electron microscope observation with molecular knife, screening
Go out 6-8 lamellar graphenes；.
Step 4: the 6-8 lamellars graphene that step 3 filters out is mixed in proportion with diamond, in 100-200Pa
Vacuum condition and 600-800 DEG C of hot conditions under, at the uniform velocity stir 34-38h, get product.
Present invention also offers a kind of preparation method of low temperature lithium battery anode, carry out in accordance with the following steps：
Step a, by major ingredient, NMP and PVDF, it is added in agitator, is evacuated to -0.08~-0.09MPa, keeps true
3.5-4.5h is stirred in the case of sky, it is cmpletely dissolved, produces mixture；
Step b, SP, KS-6 and multi-layer graphene are added in the mixture obtained by step a；It is evacuated to -0.08~-
0.09MPa, keep stirring 2-4h in the case of vacuum, reach 8000~12000MPas to viscosity, produce anode sizing agent.
The beneficial effects of the invention are as follows：
Anode additive in the present invention is added by solid-state prepared by multi-layer graphene and diamond after chemical reaction
Add agent material, the number of plies of multi-layer graphene is 6-8 layers, and the reaction ratio of multi-layer graphene and diamond is 5：1, multi-layer graphene
Added with 2-7% ratio in positive electrode, realize in the relatively low environment of temperature, get through battery electrolyte low-temperature setting and block up
The electronics and ion channel of plug, increase the purpose of ion activity, so that battery can preferably work when low temperature, most
Low to be worked in the environment of -40 DEG C, the moment for avoiding lithium battery from being opened in electronic product burns, and increase lithium battery is in low temperature
The security to be worked under environment.
Above description of the invention is only the general introduction of technical solution of the present invention, in order to better understand the skill of the present invention
Art means, and being practiced according to the content of specification, with presently preferred embodiments of the present invention and coordinate accompanying drawing specifically below
It is bright as after.
Brief description of the drawings
Fig. 1 is the structural representation of the multi-layer graphene of the present invention；
Each several part mark is as follows in accompanying drawing：
Multi-layer graphene 100, flake graphite alkene 101, carbon atom 102 and diamond 103.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.Without departing substantially from spirit of the invention
In the case of essence, the modifications or substitutions made to the inventive method, step or condition, the protection model of the present invention is belonged to
Enclose.
A kind of low temperature lithium battery anode and preparation method thereof, including major ingredient, solvent and additive, the major ingredient are ferric phosphate
Lithium or ternary, the solvent are NMP, and the additive includes PVDF, SP, KS-6 and multi-layer graphene 100；
The weight percentage of each component is as follows：The major ingredient is 40-46%, the NMP is 47-50%, the PVDF
For 2-3%, the SP be 1-2%, the KS-6 is 1-2% and the multi-layer graphene is 2-7%；
As shown in figure 1, the multi-layer graphene 100 includes multilayer chip graphene 101 and diamond 103, the Buddha's warrior attendant
Stone 103 is located between adjacent two layers of multilayer chip graphene, the carbon of the diamond and described multilayer chip graphene
Atom 102 corresponds；
The weight ratio of the multilayer chip graphene 101 and the diamond 103 is (4-6)：1；
The multilayer chip graphene is 6-8 lamellar graphenes, and every layer of thickness of the multilayer chip graphene is
0.3-0.7nm, the interlamellar spacing of the adjacent two layers of the multilayer chip graphene 101 is 0.1-0.5nm；
The diamond 103 is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.7-1.6nm.
Embodiment 1：The major ingredient is 40%, the NMP is 49%, the PVDF is 2.5%, the SP is 2%, described
KS-6 is 1.5% and the multi-layer graphene is 5%；
The weight ratio of the multilayer chip graphene and the diamond is 5：1；
The number of plies of the multilayer chip graphene is 8 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.5nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.3nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.9nm.
Embodiment 2：The major ingredient is 43%, the NMP is 50%, the PVDF is 2%, the SP is 1.2%, described
KS-6 is 1.8% and the multi-layer graphene is 2%；
The weight ratio of the multilayer chip graphene and the diamond is 4：1；
The number of plies of the multilayer chip graphene is 8 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.3nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.4nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 1.2nm.
Embodiment 3：The major ingredient is 44%, the NMP is 48%, the PVDF is 2.6%, the SP is 1.4%, institute
State that KS-6 is 1% and the multi-layer graphene is 3%；
The weight ratio of the multilayer chip graphene and the diamond is 6：1；
The number of plies of the multilayer chip graphene is 7 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.6nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.5nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 1.6nm.
Embodiment 4：The major ingredient is 41%, the NMP is 47%, the PVDF is 2%, the SP is 1%, described
KS-6 is 2% and the multi-layer graphene is 7%；
The weight ratio of the multilayer chip graphene and the diamond is 4.5：1；
The number of plies of the multilayer chip graphene is 6 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.7nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.2nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 1.0nm.
Embodiment 5：The major ingredient is 46%, the NMP is 47%, the PVDF is 3%, the SP is 1%, described
KS-6 is 1% and the multi-layer graphene is 2%；
The weight ratio of the multilayer chip graphene and the diamond is 5.5：1；
The number of plies of the multilayer chip graphene is 6 lamellar graphenes, every layer of thickness of the multilayer chip graphene
Spend for 0.4nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.1nm；
The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.7nm.
Embodiments of the invention 1 are carried out in accordance with the following steps to the preparation method of the multi-layer graphene described in embodiment 5：
Step 1: multilayer chip graphene is prepared using chemical deposition：With cathode-ray on silica substrate surface
One layer of nickel metal layer is deposited, the thickness of the nickel metal layer is 200-400nm；
Step 2: be passed through in the tube furnace of 950-1150 DEG C of temperature methane, hydrogen and ammonia composition gaseous mixture and
Common graphite powder, room temperature is cooled within 100ms, obtains multilayer chip graphene, the layer of multilayer chip graphene described herein
Number is 3-12 layers；
Step 3: more than 100,000 grades under cleanliness factor environment, by being peeled off after electron microscope observation with molecular knife, screening
Go out 6-8 lamellar graphenes；.
Step 4: the 6-8 lamellars graphene that step 3 filters out is mixed in proportion with diamond, in 100-200Pa
Vacuum condition and 600-800 DEG C of hot conditions under, at the uniform velocity stir 34-38h, get product.
In the present embodiment preferably, the thickness of the nickel metal layer is 300nm.
Embodiments of the invention 1 enter in accordance with the following steps to the preparation method of the low temperature lithium battery anode described in embodiment 5
OK：
Step a, by major ingredient, NMP and PVDF, it is added in agitator, is evacuated to -0.08~-0.09MPa, keeps true
3.5-4.5h is stirred in the case of sky, it is cmpletely dissolved, produces mixture；
Step b, SP, KS-6 and multi-layer graphene are added in the mixture obtained by step a；It is evacuated to -0.08~-
0.09MPa, keep stirring 2-4h in the case of vacuum, reach 8000~12000MPas to viscosity, produce anode sizing agent.
Multi-layer graphene is added in positive electrode with 2-7% ratio in the present invention, is realized in the relatively low environment of temperature,
The electronics and ion channel got through battery electrolyte low-temperature setting and blocked, increase the purpose of ion activity, so that battery exists
Can preferably it be worked when low temperature, it is minimum to be worked in the environment of -40 DEG C, avoid lithium battery from being opened in electronic product
Moment burn, the security that works at low ambient temperatures of increase lithium battery.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.Here without exhaustive.And the obvious changes or variations thus extended out is still in the protection of the invention
Among scope.
Claims (4)
- A kind of 1. low temperature lithium battery anode, it is characterised in that：Including major ingredient, solvent and additive, the major ingredient is LiFePO4 Or ternary, the solvent are NMP, the additive includes PVDF, SP, KS-6 and multi-layer graphene；The weight percentage of each component is as follows：The major ingredient is 40-46%, the NMP is 47-50%, the PVDF is 2- 3%th, the SP is 1-2%, the KS-6 is 1-2% and the multi-layer graphene is 2-7%；The multi-layer graphene includes multilayer chip graphene and diamond, and the diamond is located at the phase of multilayer chip graphene Between adjacent two layers, the carbon atom of the diamond and described multilayer chip graphene corresponds；The weight ratio of the multilayer chip graphene and the diamond is (4-6)：1；The multilayer chip graphene is 6-8 lamellar graphenes, and every layer of thickness of the multilayer chip graphene is 0.3- 0.7nm, the interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.1-0.5nm；The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.7-1.6nm.
- 2. low temperature lithium battery according to claim 1 is just, it is characterised in that：The multilayer chip graphene and the Buddha's warrior attendant The weight ratio of stone is 5：1；The number of plies of the multilayer chip graphene is 8 lamellar graphenes, and every layer of thickness of the multilayer chip graphene is 0.5nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.3nm；The diamond is Spherical Carbon, and the particle diameter of the Spherical Carbon is 0.9nm.
- 3. low temperature lithium battery anode according to claim 1, it is characterised in that：The preparation method of the multi-layer graphene, Comprise the following steps：Step 1: multilayer chip graphene is prepared using chemical deposition：Deposited with cathode-ray on silica substrate surface One layer of nickel metal layer, the thickness of the nickel metal layer is 200-400nm；Step 2: methane, the gaseous mixture of hydrogen and ammonia composition and common are passed through in the tube furnace of 950-1150 DEG C of temperature Graphite powder, room temperature is cooled within 100ms, obtains multilayer chip graphene, the number of plies of multilayer chip graphene described herein is 3-12 layers；Step 3: more than 100,000 grades under cleanliness factor environment, by being peeled off after electron microscope observation with molecular knife, 6- is filtered out 8 lamellar graphenes；Step 4: the 6-8 lamellars graphene that step 3 filters out is mixed in proportion with diamond, in the true of 100-200Pa Under empty condition and 600-800 DEG C of hot conditions, 34-38h is at the uniform velocity stirred, is got product.
- A kind of 4. preparation method of the low temperature lithium battery anode containing described in claim 1, it is characterised in that：In accordance with the following steps Carry out：Step a, by major ingredient, NMP and PVDF, it is added in agitator, is evacuated to -0.08~-0.09MPa, keeps vacuum In the case of stir 3.5-4.5h, it is cmpletely dissolved, produce mixture；Step b, SP, KS-6 and multi-layer graphene are added in the mixture obtained by step a；It is evacuated to -0.08~- 0.09MPa, keep stirring 2-4h in the case of vacuum, reach 8000-12000MPas to viscosity, produce anode sizing agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108470913A (en) * | 2018-05-24 | 2018-08-31 | 江苏芯界新能源科技有限公司 | A kind of High Temperature Lithium Cell anode and preparation method thereof |
| CN108682789A (en) * | 2018-06-01 | 2018-10-19 | 江苏芯界新能源科技有限公司 | A kind of low temperature lithium battery anode and preparation method thereof |
| CN108736066A (en) * | 2018-05-24 | 2018-11-02 | 江苏芯界新能源科技有限公司 | A kind of low temperature lithium battery electrolytes and preparation method thereof |
-
2017
- 2017-07-21 CN CN201710600465.4A patent/CN107482168A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108470913A (en) * | 2018-05-24 | 2018-08-31 | 江苏芯界新能源科技有限公司 | A kind of High Temperature Lithium Cell anode and preparation method thereof |
| CN108736066A (en) * | 2018-05-24 | 2018-11-02 | 江苏芯界新能源科技有限公司 | A kind of low temperature lithium battery electrolytes and preparation method thereof |
| CN108682789A (en) * | 2018-06-01 | 2018-10-19 | 江苏芯界新能源科技有限公司 | A kind of low temperature lithium battery anode and preparation method thereof |
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Application publication date: 20171215 Assignee: Kunshan Jin Xin new energy Limited by Share Ltd Assignor: Kunshan state is the new energy power battery Co., Ltd. Contract record no.: 2018320010058 Denomination of invention: Low-temperature lithium battery positive electrode and production method thereof License type: Exclusive License Record date: 20181114 |
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Application publication date: 20171215 |