CN106058197A - Novel battery cathode material and preparation method thereof - Google Patents
Novel battery cathode material and preparation method thereof Download PDFInfo
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- CN106058197A CN106058197A CN201610595656.1A CN201610595656A CN106058197A CN 106058197 A CN106058197 A CN 106058197A CN 201610595656 A CN201610595656 A CN 201610595656A CN 106058197 A CN106058197 A CN 106058197A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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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- 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
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Abstract
The invention discloses a novel battery cathode material and a preparation method thereof. The novel battery cathode material is prepared from, by weight, 40-50 parts of graphene oxide, 40-50 parts of tin tetrachloride, 15-25 parts of modified diatomite, 6-8 parts of polyvinylidene fluoride and 6-8 parts of glycerin. The preparation method of the modified diatomite includes steps: step S1, adding four to five times of water to dilute concentrated hydrochloric acid to obtain diluted hydrochloric acid, spraying the diluted hydrochloric acid while stirring diatomite, and standing in a closed environment for 10-20min after acid spraying is finished, wherein per gram of diatomite requires spraying of 8-12ml of diluted hydrochloric acid; step S2, adding N-methyl pyrrolidone, well stirring, and reacting for 2-3h at 50-60 DEG C, wherein per gram of diatomite requires addition of 6-8ml of N-methyl pyrrolidone; step S3, drying the diatomite obtained at the step S2 at 75-85 DEG C, and grinding to obtain fine powder being 400-600 meshes in particle size. The novel battery cathode material has advantages of high charge-discharge efficiency, excellent cycle performance, simplicity of a preparation process and low cost of raw materials.
Description
Technical field
The invention belongs to field of new, be specifically related to a kind of battery cathode new material and preparation method thereof.
Background technology
Negative pole refers to one end that in power supply, current potential is relatively low.In galvanic element, refer to the electrode of Oxidation, in cell reaction
Write on the left side.From the point of view of physical angle, it is the pole that in circuit, electronics flows out.And negative material, then refer to battery is constituted bear
The raw material of pole, the most common negative material has carbon negative pole material, tin base cathode material, lithium-containing transition metal nitride negative pole material
Material, alloy type negative material and nanoscale negative material.
One of lithium battery currently the most important ones battery, its be a class by lithium metal or lithium alloy be negative material, use non-
The battery of non-aqueous electrolytic solution.The negative pole of lithium ion battery be by negative electrode active material material with carbon element or non-carbon material, binding agent and
Additive is mixed and made into pasty state adhesive uniform application in Copper Foil both sides, and drying, rolling form.Lithium ion battery success
Make, it is critical only that the negative material that can prepare reversibly de-/embedding lithium ion.In general, a kind of good bearing is selected
Pole material should follow following principle: specific energy is high；The electrode potential of lithium electrode relatively is low；Discharge and recharge reaction good reversibility；With electricity
The compatibility solving liquid and binding agent is good；The little (< 10m of specific surface area2/ g), the high (> 2.0g/cm of true density3)；Size in process of intercalation
And good mechanical stability；Aboundresources, cheap；Stable in the air, have no side effect.
The exploitation of high-performance negative material contributes to promoting the update of lithium battery.
Summary of the invention
It is an object of the invention to provide a kind of battery cathode new material and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of battery cathode new material, is made by the raw material of following weight portion: graphene oxide, 40～50 parts；Tetrachloro
Change stannum, 40～50 parts；Modification infusorial earth, 15～25 parts；Kynoar, 6～8 parts；Glycerol, 6～8 parts；
The preparation method of described modification infusorial earth comprises the steps:
Step S1, takes concentrated hydrochloric acid and adds 4～5 times of prepared dilute hydrochloric acid of water dilution, while stir kieselguhr limit sprinkling dilute hydrochloric acid, and every gram
Kieselguhr sprays 8～12ml dilute hydrochloric acid, and spray acid terminates to be placed in closed environment vexed system 10～20 minutes；Step S2, adds
N-Methyl pyrrolidone, stirs and reacts 2～3 hours in 50～60 DEG C after stirring, and every gram of kieselguhr adds 6～8ml N-first
Base ketopyrrolidine；Step S3, grinding to form particle diameter after being dried in 75～85 DEG C by step S2 gained kieselguhr is 400～600 purposes
Fine powder.
Further, described battery cathode new material is made by the raw material of following weight portion: graphene oxide, and 45
Part；Butter of tin, 45 parts；Modification infusorial earth, 20 parts；Kynoar, 7 parts；Glycerol, 7 parts.
Further, described battery cathode new material is made by the raw material of following weight portion: graphene oxide, and 40
Part；Butter of tin, 40 parts；Modification infusorial earth, 15 parts；Kynoar, 6 parts；Glycerol, 6 parts.
Further, described battery cathode new material is made by the raw material of following weight portion: graphene oxide, and 50
Part；Butter of tin, 50 parts；Modification infusorial earth, 25 parts；Kynoar, 8 parts；Glycerol, 8 parts.
Further, the preparation method of described modification infusorial earth comprises the steps: step S1, takes concentrated hydrochloric acid and adds 4.5 times
Water dilution prepares dilute hydrochloric acid, while stir kieselguhr limit to spray dilute hydrochloric acid, every gram of kieselguhr sprays 10ml dilute hydrochloric acid, after spray acid terminates
It is placed in vexed system 15 minutes in closed environment；Step S2, adds N-Methyl pyrrolidone, stirs after stirring in 55 DEG C of reactions
2.5 hours, every gram of kieselguhr added 7ml N-Methyl pyrrolidone；Step S3, by step S2 gained kieselguhr in 80 DEG C of drying
After grind to form the fine powder that particle diameter is 500 mesh.
The preparation method of above-mentioned battery cathode new material, comprises the steps:
Step S1, ball milling graphene oxide: it is 400～600 mesh that graphene oxide is milled to particle diameter；
Step S2, prepare butter of tin solution: with water as solvent, and butter of tin is configured to mass fraction 60～70%
Solution；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to quality
Mark is the Kynoar solution of 16～20%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, modification infusorial earth, Kynoar solution and
Glycerol mix and blend, rotating speed 320～340rpm, stirs 6～10 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, place at 50～60 DEG C
10～12 hours, it is subsequently placed in the water of 8～12 DEG C cooling, takes out, after drying at 90～110 DEG C, carry out cutting, finally at argon
Under gas shielded atmosphere, 600～700 DEG C sinter 2～3 hours, to obtain final product.
Further, during coating sintering, mixed material step S4 obtained is coated on round copper sheet, places at 55 DEG C
11 hours, it is subsequently placed in the water of 10 DEG C cooling, takes out, after drying at 100 DEG C, carry out cutting, finally under argon atmosphere
650 DEG C sinter 2.5 hours.
Advantages of the present invention:
The battery cathode new material efficiency for charge-discharge that the present invention provides is high, good cycle, and preparation technology is simple, and raw material becomes
This is cheap, compared with prior art has prominent substantive distinguishing features and significantly progress.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit the present invention with this and protect model
Enclose.Although the present invention being explained in detail with reference to preferred embodiment, it will be understood by those within the art that, can be right
Technical scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
In the present invention, graphene oxide uses the Hummers method of improvement to prepare, and sees document Hummers, W.S.,
Jr.；Offeman,R.E.J.Am.Chem.Soc.1958,80,1339.
Embodiment 1: the preparation of cell negative electrode material
Parts by weight of raw materials compares: graphene oxide, 45 parts；Butter of tin, 45 parts；Modification infusorial earth, 20 parts；Polyvinylidene fluoride
Alkene, 7 parts；Glycerol, 7 parts.
The preparation method of modification infusorial earth comprises the steps:
Step S1, takes concentrated hydrochloric acid and adds 4.5 times of prepared dilute hydrochloric acid of water dilution, while stir kieselguhr limit sprinkling dilute hydrochloric acid, and every gram
Kieselguhr sprays 10ml dilute hydrochloric acid, and spray acid terminates to be placed on vexed system 15 minutes in closed environment；Step S2, adds N-methyl pyrrole
Pyrrolidone, stirs and reacts 2.5 hours in 55 DEG C after stirring, and every gram of kieselguhr adds 7ml N-Methyl pyrrolidone；Step
S3, grinds to form, after being dried in 80 DEG C by step S2 gained kieselguhr, the fine powder that particle diameter is 500 mesh.
Preparation method:
Step S1, ball milling graphene oxide: it is 500 mesh that graphene oxide is milled to particle diameter；
Step S2, prepares butter of tin solution: with water as solvent, butter of tin is configured to the molten of mass fraction 65%
Liquid；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to quality
Mark is the Kynoar solution of 18%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, modification infusorial earth, Kynoar solution and
Glycerol mix and blend, rotating speed 330rpm, stirs 8 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, at 55 DEG C, place 11 little
Time, it is subsequently placed in the water of 10 DEG C cooling, takes out, after drying at 100 DEG C, carry out cutting, finally under argon atmosphere 650
DEG C sintering 2.5 hours, to obtain final product.
Embodiment 2: the preparation of cell negative electrode material
Parts by weight of raw materials compares: graphene oxide, 40 parts；Butter of tin, 40 parts；Modification infusorial earth, 15 parts；Polyvinylidene fluoride
Alkene, 6 parts；Glycerol, 6 parts.
The preparation method of modification infusorial earth comprises the steps:
Step S1, takes concentrated hydrochloric acid and adds 4.5 times of prepared dilute hydrochloric acid of water dilution, while stir kieselguhr limit sprinkling dilute hydrochloric acid, and every gram
Kieselguhr sprays 10ml dilute hydrochloric acid, and spray acid terminates to be placed on vexed system 15 minutes in closed environment；Step S2, adds N-methyl pyrrole
Pyrrolidone, stirs and reacts 2.5 hours in 55 DEG C after stirring, and every gram of kieselguhr adds 7ml N-Methyl pyrrolidone；Step
S3, grinds to form, after being dried in 80 DEG C by step S2 gained kieselguhr, the fine powder that particle diameter is 500 mesh.
Preparation method:
Step S1, ball milling graphene oxide: it is 500 mesh that graphene oxide is milled to particle diameter；
Step S2, prepares butter of tin solution: with water as solvent, butter of tin is configured to the molten of mass fraction 65%
Liquid；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to quality
Mark is the Kynoar solution of 18%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, modification infusorial earth, Kynoar solution and
Glycerol mix and blend, rotating speed 330rpm, stirs 8 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, at 55 DEG C, place 11 little
Time, it is subsequently placed in the water of 10 DEG C cooling, takes out, after drying at 100 DEG C, carry out cutting, finally under argon atmosphere 650
DEG C sintering 2.5 hours, to obtain final product.
Embodiment 3: the preparation of cell negative electrode material
Parts by weight of raw materials compares: graphene oxide, 50 parts；Butter of tin, 50 parts；Modification infusorial earth, 25 parts；Polyvinylidene fluoride
Alkene, 8 parts；Glycerol, 8 parts.
The preparation method of modification infusorial earth comprises the steps:
Step S1, takes concentrated hydrochloric acid and adds 4.5 times of prepared dilute hydrochloric acid of water dilution, while stir kieselguhr limit sprinkling dilute hydrochloric acid, and every gram
Kieselguhr sprays 10ml dilute hydrochloric acid, and spray acid terminates to be placed on vexed system 15 minutes in closed environment；Step S2, adds N-methyl pyrrole
Pyrrolidone, stirs and reacts 2.5 hours in 55 DEG C after stirring, and every gram of kieselguhr adds 7ml N-Methyl pyrrolidone；Step
S3, grinds to form, after being dried in 80 DEG C by step S2 gained kieselguhr, the fine powder that particle diameter is 500 mesh.
Preparation method:
Step S1, ball milling graphene oxide: it is 500 mesh that graphene oxide is milled to particle diameter；
Step S2, prepares butter of tin solution: with water as solvent, butter of tin is configured to the molten of mass fraction 65%
Liquid；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to quality
Mark is the Kynoar solution of 18%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, modification infusorial earth, Kynoar solution and
Glycerol mix and blend, rotating speed 330rpm, stirs 8 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, at 55 DEG C, place 11 little
Time, it is subsequently placed in the water of 10 DEG C cooling, takes out, after drying at 100 DEG C, carry out cutting, finally under argon atmosphere 650
DEG C sintering 2.5 hours, to obtain final product.
Embodiment 4: comparative example, kieselguhr is the most modified
Parts by weight of raw materials compares: graphene oxide, 45 parts；Butter of tin, 45 parts；500 mesh kieselguhr, 20 parts；Polyvinylidene fluoride
Alkene, 7 parts；Glycerol, 7 parts.
Preparation method:
Step S1, ball milling graphene oxide: it is 500 mesh that graphene oxide is milled to particle diameter；
Step S2, prepares butter of tin solution: with water as solvent, butter of tin is configured to the molten of mass fraction 65%
Liquid；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to quality
Mark is the Kynoar solution of 18%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, 500 mesh kieselguhr, Kynoar solution
With glycerol mix and blend, rotating speed 330rpm, stir 8 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, at 55 DEG C, place 11 little
Time, it is subsequently placed in the water of 10 DEG C cooling, takes out, after drying at 100 DEG C, carry out cutting, finally under argon atmosphere 650
DEG C sintering 2.5 hours, to obtain final product.
Embodiment 5: effect example
The material using new prestige battery test system to prepare embodiment 1～4 carries out constant current charge-discharge cycle performance test,
Charging and discharging currents density is 0.1mA/cm2, voltage range is 0.2-1.5V (Li+/Li).Reversible capacity, efficiency for charge-discharge first
As shown in the table with the reversible capacity after 50 charge and discharge cycles, efficiency for charge-discharge:
The above results shows, the battery cathode new material efficiency for charge-discharge that the present invention provides is high, good cycle, prepares work
Skill is simple, low raw-material cost, compared with prior art has prominent substantive distinguishing features and significantly progress.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit the protection of the present invention with this
Scope.It will be understood by those within the art that, technical scheme can be modified or equivalent,
Essence and protection domain without deviating from technical solution of the present invention.
Claims (7)
1. a battery cathode new material, it is characterised in that made by the raw material of following weight portion: graphene oxide, 40～
50 parts；Butter of tin, 40～50 parts；Modification infusorial earth, 15～25 parts；Kynoar, 6～8 parts；Glycerol, 6～8 parts；
The preparation method of described modification infusorial earth comprises the steps:
Step S1, takes concentrated hydrochloric acid and adds 4～5 times of prepared dilute hydrochloric acid of water dilution, while stir kieselguhr limit to spray dilute hydrochloric acid, every gram of diatom
Soil sprays 8～12ml dilute hydrochloric acid, and spray acid terminates to be placed in closed environment vexed system 10～20 minutes；Step S2, adds N-first
Base ketopyrrolidine, stirs and reacts 2～3 hours in 50～60 DEG C after stirring, and every gram of kieselguhr adds 6～8ml N-methyl pyrroles
Pyrrolidone；Step S3, grinds to form, after being dried in 75～85 DEG C by step S2 gained kieselguhr, the fine powder that particle diameter is 400～600 mesh.
Battery cathode new material the most according to claim 1, it is characterised in that made by the raw material of following weight portion:
Graphene oxide, 45 parts；Butter of tin, 45 parts；Modification infusorial earth, 20 parts；Kynoar, 7 parts；Glycerol, 7 parts.
Battery cathode new material the most according to claim 1, it is characterised in that made by the raw material of following weight portion:
Graphene oxide, 40 parts；Butter of tin, 40 parts；Modification infusorial earth, 15 parts；Kynoar, 6 parts；Glycerol, 6 parts.
Battery cathode new material the most according to claim 1, it is characterised in that made by the raw material of following weight portion:
Graphene oxide, 50 parts；Butter of tin, 50 parts；Modification infusorial earth, 25 parts；Kynoar, 8 parts；Glycerol, 8 parts.
5. according to the arbitrary described battery cathode new material of Claims 1 to 4, it is characterised in that the system of described modification infusorial earth
Preparation Method comprises the steps: step S1, takes concentrated hydrochloric acid and adds 4.5 times of prepared dilute hydrochloric acid of water dilution, sprays while stir kieselguhr limit
Dilute hydrochloric acid, every gram of kieselguhr sprays 10ml dilute hydrochloric acid, and spray acid terminates to be placed on vexed system 15 minutes in closed environment；Step S2, then
Adding N-Methyl pyrrolidone, stir and react 2.5 hours in 55 DEG C after stirring, every gram of kieselguhr adds 7ml N-methyl pyrrole
Pyrrolidone；Step S3, grinds to form, after being dried in 80 DEG C by step S2 gained kieselguhr, the fine powder that particle diameter is 500 mesh.
6. the preparation method of the arbitrary described battery cathode new material of Claims 1 to 4, it is characterised in that comprise the steps:
Step S1, ball milling graphene oxide: it is 400～600 mesh that graphene oxide is milled to particle diameter；
Step S2, prepares butter of tin solution: with water as solvent, butter of tin is configured to mass fraction 60～70% molten
Liquid；
Step S3, prepares Kynoar solution: with dimethyl acetylamide as solvent, Kynoar is configured to mass fraction
It is the Kynoar solution of 16～20%；
Step S4, mix and blend: by graphene oxide, butter of tin solution, modification infusorial earth, Kynoar solution and glycerol
Mix and blend, rotating speed 320～340rpm, stirs 6～10 minutes；
Step S5, coating sintering: mixed material step S4 obtained is coated on round copper sheet, at 50～60 DEG C place 10～
12 hours, it is subsequently placed in the water of 8～12 DEG C cooling, takes out, carry out cutting after drying at 90～110 DEG C, finally protect at argon
Protect under atmosphere 600～700 DEG C to sinter 2～3 hours, to obtain final product.
Preparation method the most according to claim 6, it is characterised in that: during coating sintering, the mixture that step S4 is obtained
Material is coated on round copper sheet, places 11 hours, be subsequently placed in the water of 10 DEG C cooling at 55 DEG C, takes out, after drying at 100 DEG C
Carry out cutting, finally under argon atmosphere 650 DEG C sinter 2.5 hours.
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| US7335321B1 (en) * | 1999-11-29 | 2008-02-26 | Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. | Films for electrochemical components and method for production thereof |
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| CN103022454A (en) * | 2012-11-28 | 2013-04-03 | 上海锦众信息科技有限公司 | Preparation method of tin-carbon composite negative electrode material |
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| US7335321B1 (en) * | 1999-11-29 | 2008-02-26 | Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. | Films for electrochemical components and method for production thereof |
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