CN108807932A - Cathode material and preparation method thereof for graphene battery - Google Patents
Cathode material and preparation method thereof for graphene battery Download PDFInfo
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- CN108807932A CN108807932A CN201810669859.XA CN201810669859A CN108807932A CN 108807932 A CN108807932 A CN 108807932A CN 201810669859 A CN201810669859 A CN 201810669859A CN 108807932 A CN108807932 A CN 108807932A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active 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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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Abstract
The cathode material and preparation method thereof that the invention discloses a kind of for graphene battery not only ensure that the height ratio capacity of cathode material by Doped with Titanium, platinum, tungsten, molybdenum, lithium in electrically conductive graphite, additionally it is possible to improve the electric conductivity of cathode material；Cathode material is by three structure compositions, it is followed successively by base material from the inside to the outside, electrically conductive graphite, titanium, platinum, tungsten, molybdenum, lithium mixture, graphene, the cathode material conductivity of the structure is high, specific capacity is big, and high cathode specific capacity is kept after multiple charge/discharge cycle, to improve the cycle life of graphene battery.In addition, low raw-material cost simple for process provided by the present invention for the preparation method of the cathode material of graphene battery, is suitble to industrialized production.
Description
Technical field
The present invention relates to field of batteries, especially a kind of cathode materials and preparation method thereof for graphene battery.
Background technology
Graphene is a kind of cellular flat film formed with sp2 hybrid forms by carbon atom, is there are one a kind of
The quasi- two-dimensional material of atomic layer level thickness does monoatomic layer graphite so being called.Univ Manchester UK physicist An Delie
Lid nurse and Constantine's Nuo Woxiao loves are isolated graphene with micromechanics stripping method success from graphite, therefore are obtained jointly
Obtain Nobel Prize in physics in 2010.The method of the common power production of graphene is mechanical stripping method, oxidation-reduction method, film
Production method is chemical vapour deposition technique.Due to its very good intensity, flexible, conductive, heat conduction, optical characteristics, in physics
The fields such as, materialogy, electronic information, computer, aerospace are obtained for significant progress.
In terms of energy storage, graphene also obtains the research and development energetically of scientific research personnel in recent years.Two-dimentional membrane material is as graphene
A kind of form that functionalization may be implemented also obtains industry and studies energetically, nowadays the closelypacked graphene film table of LBL self-assembly
High conductivity, high intensity and the excellent toughness revealed is also that industry is extremely paid close attention to.But graphene is for making at present
When electrode in battery, specific capacity is low, and cycle life is poor.
Invention content
In view of this, the object of the present invention is to provide a kind of cathode material of graphene battery and preparation method thereof, specific volume
Amount is high, and battery cycle life is long.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of cathode material for graphene battery includes the raw material of following parts by weight：
Preferably, the base material is carbon-point, graphite rod or tungsten bar.
The present invention also provides a kind of preparation methods of above-mentioned cathode material for graphene battery, including following step
Suddenly：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to substrate surface, just cathode substrate is obtained after dry；
B) it by graphite oxidation at graphite oxide, and will be dispersed in deionization in graphite oxide, reducing agent be added, obtains pre-
Reduced graphene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Preferably, the reducing agent is vitamin C, hydrazine hydrate.
Preferably, the mass ratio of the reducing agent and the graphite is 1:2~3.
Preferably, the graphite oxidation is Hummers methods at the preparation method of graphite oxide solution.
The cathode material and preparation method thereof that the present invention provides a kind of for graphene battery, by electrically conductive graphite
Doped with Titanium, platinum, tungsten, molybdenum, lithium not only ensure that the height ratio capacity of cathode material, additionally it is possible to improve the electric conductivity of cathode material；
Cathode material is followed successively by base material, electrically conductive graphite, titanium, platinum, tungsten, molybdenum, lithium mixture, graphite from the inside to the outside by three structure compositions
The cathode material conductivity of alkene, the structure is high, and specific capacity is big, and high cathode specific capacity is kept after multiple charge/discharge cycle,
To improve the cycle life of graphene battery.In addition, the preparation of the cathode material provided by the present invention for graphene battery
Method and process is simple, low raw-material cost, is suitble to industrialized production.
Specific implementation mode
A kind of cathode material for graphene battery provided by the invention, includes the raw material of following parts by weight：
In above-mentioned technical proposal, by Doped with Titanium, platinum, tungsten, molybdenum, lithium in electrically conductive graphite, cathode material not only ensure that
Height ratio capacity, additionally it is possible to improve the electric conductivity of cathode material；Cathode material is followed successively by from the inside to the outside by three structure compositions
The cathode material conductivity of base material, electrically conductive graphite, titanium, platinum, tungsten, molybdenum, lithium mixture, graphene, the structure is high, and specific capacity is big,
High cathode specific capacity is kept after multiple charge/discharge cycle, to improve the cycle life of graphene battery.
Base material plays conductive effect in graphite cell.In an embodiment of the present invention, base material be carbon-point, graphite rod or
Tungsten bar.
In the present invention, the parts by weight of base material are 80~100 parts；In an embodiment of the present invention, the parts by weight of base material
Number is 85~95 parts；In other embodiments, the parts by weight of base material are 88~92 parts.
Polyimides conducting resinl enables to carbon black, titanium, platinum, tungsten, molybdenum, lithium to be firmly adhered on base material, improves cathode
The cycle performance and security performance of material, improve the service life cycle of graphene battery.In the present invention, polyimides is conductive
The parts by weight of glue are 2~3 parts；In an embodiment of the present invention, the parts by weight of polyimides conducting resinl are 2.2~2.8 parts；
In other embodiments, the parts by weight of polyimides conducting resinl are 2.4~2.6 parts.
Graphene is used to improve the ratio energy and battery cycle life of graphene battery.In the present invention, the weight of graphene
It is 1~2 part to measure number；In an embodiment of the present invention, the parts by weight of graphene are 1.2~1.8 parts；In other embodiment
In, the parts by weight of graphene are 1.4~1.6 parts.
Carbon black, titanium, platinum, tungsten, molybdenum, lithium improve the cycle life of battery for reducing graphene and base material contact resistance.?
In the present invention, the parts by weight of carbon black are 1~2 part；In an embodiment of the present invention, the parts by weight of carbon black are 1.2~1.8
Part；In other embodiments, the parts by weight of carbon black are 1.4~1.6 parts.
In the present invention, the parts by weight of titanium are 0.1~0.2 part；In an embodiment of the present invention, the parts by weight of titanium are
0.12~0.17 part；In other embodiments, the parts by weight of titanium are 0.14~0.16 part.
In the present invention, the parts by weight of platinum are 0.1~0.2 part；In an embodiment of the present invention, the parts by weight of platinum are
0.11~0.18 part；In other embodiments, the parts by weight of platinum are 0.13~0.15 part.
In the present invention, the parts by weight of tungsten are 0.05~0.08 part；In an embodiment of the present invention, the parts by weight of tungsten
It is 0.055~0.075 part；In other embodiments, the parts by weight of tungsten are 0.06~0.07 part.
In the present invention, the parts by weight of molybdenum are 0.02~0.03 part；In an embodiment of the present invention, the parts by weight of molybdenum
It is 0.023~0.027 part；In other embodiments, the parts by weight of molybdenum are 0.024~0.026 part.
In the present invention, the parts by weight of lithium are 0.1~0.2 part；In an embodiment of the present invention, the parts by weight of lithium are
0.12~0.17 part；In other embodiments, the parts by weight of lithium are 0.13~0.15 part.
In an embodiment of the present invention, base material is carbon-point, graphite rod or tungsten bar.
The present invention also provides a kind of preparation methods of above-mentioned cathode material for graphene battery, including following step
Suddenly：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to substrate surface, just cathode substrate is obtained after dry；
B) it by graphite oxidation at graphite oxide, and will be dispersed in deionization in graphite oxide, reducing agent be added, obtains pre-
Reduced graphene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
It is conductive by first coating carbon black, titanium, platinum, tungsten, molybdenum, lithium and polyimides in substrate surface in above-mentioned technical proposal
The mixture of glue, then prereduction graphene solution is coated on first cathode substrate surface, so that it is steady to obtain cathode material structure
Qualitative good, the contact resistance between graphene and base material is low, and conductivity is high, and specific capacity is big, is protected after multiple charge/discharge cycle
High cathode specific capacity is held, to improve the cycle life of graphene battery.In addition, provided by the present invention for graphene battery
Cathode material preparation method it is simple for process, low raw-material cost, be suitble to industrialized production.
In an embodiment of the present invention, reducing agent is vitamin C or hydrazine hydrate.
In an embodiment of the present invention, the mass ratio of reducing agent and graphite is 1:2~3.
In an embodiment of the present invention, graphite oxidation is Hummers methods at the preparation method of graphite oxide solution.
In an embodiment of the present invention, Hummers methods are to weigh 5g grain sizes as 300 mesh crystalline flake graphites and 2gNaNO3It carries out
It mitigates, the addition 120mL concentrated sulfuric acids, which are placed in ice-water bath, to be stirred, and 20gKMnO is added after 30min4, after reacting 60min, move
The 30min that enters in 40 DEG C of tepidariums that the reaction was continued, is then slowly added into 230mL deionized waters, and it is 98 DEG C to keep reaction temperature, is stirred
Appropriate hydrogen peroxide is added to bubble is not generated after mixing 5min, filters while hot, deionized water and 5% hydrochloric acid is used in combination repeatedly to be washed
It washs to neutrality, graphite oxide is fully drying to obtain in 60 DEG C of vacuum drying chambers after centrifugation.
In order to further illustrate the present invention, with reference to embodiment to provided by the invention a kind of for graphene battery
Cathode material and preparation method thereof is described in detail, but cannot they be interpreted as limiting the scope of the present invention.
Embodiment 1
It is 300 mesh crystalline flake graphites and 2gNaNO to weigh 5g grain sizes3It is mitigated, the 120mL concentrated sulfuric acids is added and are placed in ice-water bath
In stirred, 20gKMnO is added after 30min4, after reacting 60min, the reaction was continued 30min in 40 DEG C of tepidariums is moved into, so
After be slowly added to 230mL deionized waters, and it is 98 DEG C to keep reaction temperature, and appropriate hydrogen peroxide is added to not generating after stirring 5min
Bubble filters while hot, is used in combination deionized water and 5% hydrochloric acid to carry out repeatedly washing to neutrality, is dried in vacuo at 60 DEG C after centrifugation
Graphite oxide is fully drying to obtain in case.
Embodiment 2
For the cathode material of graphene battery, include the raw material of following parts by weight：
85g carbon-points, 2.2g polyimides conducting resinl, 1g carbon blacks, 0.12g titaniums, 0.11g platinum, 0.07g tungsten, 0.026g molybdenums,
0.13g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to carbon-point surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 1.5g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction stone
Black alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 3
For the cathode material of graphene battery, include the raw material of following parts by weight：
95g tungsten bars, 2.6g polyimides conducting resinl, 1.8g carbon blacks, 0.17g titaniums, 0.18g platinum, 0.055g tungsten, 0.03g molybdenums,
0.12g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to tungsten bar surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 2g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction graphite
Alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 4
For the cathode material of graphene battery, include the raw material of following parts by weight：
88g carbon-points, 2g polyimides conducting resinl, 1.2g carbon blacks, 0.2g titaniums, 0.13g platinum, 0.08g tungsten, 0.027g molybdenums,
0.17g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to carbon-point surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 2g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction graphite
Alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 5
For the cathode material of graphene battery, include the raw material of following parts by weight：
80g graphite rods, 3g polyimides conducting resinl, 1.6g carbon blacks, 0.1g titaniums, 0.2g platinum, 0.06g tungsten, 0.023g molybdenums,
0.1g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to graphite rod surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 1.8g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction stone
Black alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 6
For the cathode material of graphene battery, include the raw material of following parts by weight：
92g tungsten bars, 2.8g polyimides conducting resinl, 1.4g carbon blacks, 0.16g titaniums, 0.15g platinum, 0.075g tungsten, 0.024g
Molybdenum, 0.2g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to tungsten bar surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 1.5g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction stone
Black alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 7
For the cathode material of graphene battery, include the raw material of following parts by weight：
100g carbon-points, 2.4g polyimides conducting resinl, 2g carbon blacks, 0.14g titaniums, 0.1g platinum, 0.05g tungsten, 0.02g molybdenums,
0.15g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to carbon-point surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 1.8g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction stone
Black alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
Embodiment 8
For the cathode material of graphene battery, include the raw material of following parts by weight：
90g graphite rods, 2.5g polyimides conducting resinl, 1.5g carbon blacks, 0.15g titaniums, 0.14g platinum, 0.065g tungsten, 0.025g
Molybdenum, 0.14g lithiums；
The preparation method of cathode material for graphene battery, includes the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added to polyimides conduction
After being stirred evenly in glue, it is applied to graphite rod surface, just cathode substrate is obtained after dry；
B) it takes in graphite oxide made from 1.5g embodiments 1 and is dispersed in deionization, reducing agent is added, obtains prereduction stone
Black alkene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation,
Drying is to get the cathode material for graphene battery.
The cathode material of graphene battery made from embodiment 2~8 is subjected to conductivity test, and is put into graphene battery
In tested, record 1C for the first time discharge capacity and 500 times cycle after discharge capacity, the results are shown in Table 1.
Above description enables professional and technical personnel in the field to realize or using this to being stated in the disclosed embodiments
It is bright, it enables those skilled in the art to implement or use the present invention.Various modifications to these embodiments are to this field
It will be apparent for professional technician, the general principles defined herein can be in the spirit for not departing from the present invention
Or in the case of range, realize in other embodiments.Therefore, the present invention is not intended to be limited to these implementations shown in this article
Example, and it is to fit to the widest range consistent with principles disclosed herein and novel features.
Claims (6)
1. a kind of cathode material for graphene battery, which is characterized in that include the raw material of following parts by weight：
2. cathode material as described in claim 1, which is characterized in that the base material is carbon-point, graphite rod or tungsten bar.
3. a kind of preparation method of the cathode material as claimed in claim 1 or 2 for graphene battery, which is characterized in that
Include the following steps：
A) under the vacuum environment in vacuum glove box, carbon black, titanium, platinum, tungsten, molybdenum, lithium are added in polyimides conducting resinl
After stirring evenly, it is applied to substrate surface, just cathode substrate is obtained after dry；
B) it by graphite oxidation at graphite oxide, and will be dispersed in deionization in graphite oxide, reducing agent be added, obtains prereduction
Graphene solution；
C) the prereduction graphene solution that step b) is obtained is coated to just cathode substrate surface, and carries out laser irradiation, it is dry,
Up to the cathode material for graphene battery.
4. preparation method as claimed in claim 3, which is characterized in that the reducing agent is vitamin C or hydrazine hydrate.
5. preparation method as claimed in claim 3, which is characterized in that the mass ratio of the reducing agent and the graphite is 1:2
~3.
6. preparation method as claimed in claim 3, which is characterized in that the graphite oxidation at graphite oxide solution preparation side
Method is Hummers methods.
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