CN108022760B - A kind of graphene blended metal oxide electrode material and preparation method thereof - Google Patents
A kind of graphene blended metal oxide electrode material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of graphene blended metal oxide electrode material and preparation method thereof, is related to electrochemical material technical field.This graphene blended metal oxide electrode material, it first passes through electrolytic method and graphene is prepared, then graphene is mixed with the mixing salt solution of Ru, Sn and Co, is calcined under the conditions of 220 DEG C~300 DEG C after dry, obtains graphene/metal oxide combination electrode material.The graphene blended metal oxide electrode material is compound by introducing metal oxide and graphene progress, so that metal nanoparticle is embedded in adjacent graphene film interlayer, double layer electrodes material and fake capacitance electrode material it is reasonable compound, electric conductivity and chemical stability are good, have ideal specific capacitance.
Description
Technical field
The present invention relates to electrochemical material fields, and in particular to a kind of graphene blended metal oxide electrode material and
Preparation method.
Background technique
Supercapacitor has that high power density, charging time be short, environmentally protective and long circulation life, in electronic vapour
The fields such as vehicle, aerospace equipment and consumer electronics are with a wide range of applications.The performance of supercapacitor mainly depends on
In the selection of electrode material.Metal oxide can get very high fake capacitance based on the redox reaction of itself, wherein oxidation
Ruthenium has preferable stability and considerable fake capacitance characteristic, is acknowledged as classic electrode material, but ruthenium is expensive, limits
Make its commercialized application.Reducing cost of material and cost of manufacture containing ruthenium electrode is to realize its commercialized key.By adding
Add the 2nd constituent element that the dispersibility of ruthenium-oxide can be improved, increase the fault of construction of electrode, the activity of electrode can be effectively improved.2nd constituent element
Such as TiO2、SnO2、MnO2、Co3O4, SiO2Deng.
Graphene is a kind of carbon material of two-dimensional structure, and with ideal monoatomic layer thickness, theoretical specific surface area is high
Up to 2630m2·g-1, and electric conductivity and chemical stability are good, it is considered to be ideal electrode material for electric double layer capacitor.But model
The presence of De Huali keeps graphene easy to reunite, to reduce the specific surface area and specific capacity of graphene.
Inventor carries out that compound that nanoparticle can be made to be embedded in is adjacent the study found that introducing metal oxide and graphene
Graphene film interlayer effectively prevents graphene film from stacking again, is maintained high charge capacity to make up graphene work
For the deficiency of electrode material for super capacitor.
Summary of the invention
The purpose of the present invention is to provide a kind of composite metal oxide electrode material of graphene doping, this electrode materials
Chemical property is stablized, excellent electrical property.
Another object of the present invention is to provide a kind of preparation methods of graphene blended metal oxide electrode material.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of graphene blended metal oxide electrode material, comprising the following steps:
S1 obtains a pair of of graphite electrode and electrolyte, will be inserted into the electrolyte graphite electrode in pairs, be powered electricity
Solution obtains the graphene that electrolysis obtains；
Ru salt, Sn salt and Co salt are dissolved in solvent, obtain mixed salt solution, wherein the mixed metal by S2
In salting liquid, the atomic ratio of Ru:Sn:Co is 4:1~4:2~4；
The graphene is added in the mixed salt solution in S3, after mixing, is dried to obtain graphene-metal salt
Presoma；
S4 calcines the graphene-metal salt presoma under the conditions of 220 DEG C~300 DEG C, obtains graphene doping gold
Belong to oxide electrode material.
The present invention proposes a kind of graphene blended metal oxide electrode material, is made according to above-mentioned preparation method.
The beneficial effect of the graphene blended metal oxide electrode material of the embodiment of the present invention and preparation method thereof is:
Double layer electrodes material graphene and fake capacitance electrode material metal oxide is compound, significantly improve electrode material
Electric conductivity and chemical stability.Meanwhile it introducing metal oxide and graphene and carrying out compound to make nanoparticle insertion phase
Adjacent graphene film interlayer effectively prevents graphene film from stacking again, is maintained high charge capacity, to make up graphite
Deficiency of the alkene as electrode material for super capacitor.
Metal oxide passes through the mixing of Sn, Co and Ru, obtains ternary composite metal oxide, the knot of tissue of electrode material
Structure and chemical property are substantially change.The dispersibility for improving ruthenium-oxide forms highdensity fault of construction, effectively improves
The active dot density and electrochemical roughening degree of electrode, further increases the specific capacitance of electrode material.
In addition, preparation method of the invention is simple, and it is easily operated, it is suitable for industrialized production, there is good market to answer
Use prospect.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the shape appearance figure of graphene obtained in the embodiment of the present invention 1；
Fig. 2 is the shape appearance figure for the graphene that comparative example 4 of the present invention obtains；
Fig. 3 is the shape appearance figure of graphene made from comparative example 5 of the present invention；
Fig. 4 is the XRD spectrum of electrode material obtained by comparative example 1~3；
Fig. 5 is the XRD spectrum of electrode material obtained by Examples 1 to 3；
Fig. 6 a is the shape appearance figure of electrode material made from comparative example 1；
Fig. 6 b is the shape appearance figure of electrode material made from embodiment 1；
Fig. 6 c is the shape appearance figure of electrode material made from comparative example 2；
Fig. 6 d is the shape appearance figure of electrode material made from embodiment 2；
Fig. 6 e is the shape appearance figure of electrode material made from comparative example 3；
Fig. 6 f is the shape appearance figure of electrode material made from embodiment 3.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Graphene blended metal oxide electrode material of the embodiment of the present invention and preparation method thereof is carried out below specific
Explanation.
The embodiment of the present invention provides a kind of preparation method of graphene blended metal oxide electrode material, including following step
It is rapid:
S1 obtains a pair of of graphite electrode and electrolyte, will be inserted into the electrolyte graphite electrode in pairs, be powered electricity
Solution obtains the graphene that electrolysis obtains；
Ru salt, Sn salt and Co salt are dissolved in solvent, obtain mixed salt solution, wherein the mixed metal by S2
In salting liquid, the atomic ratio of Ru:Sn:Co is 4:1~4:2~4；
The graphene is added in the mixed salt solution in S3, after mixing, is dried to obtain graphene-metal salt
Presoma；
The graphene-metal salt presoma is calcined under the conditions of 220 DEG C~300 DEG C, obtains graphene/metal by S4
Oxide combination electrode material.
Further, in step S1, electrolyte is the NaCl solution that concentration is 18~22mg/L.It can using the electrolyte
It is tiny that particle is prepared, uniform in size, the graphene powder of shape comparison rule.
Further, after the completion of electrolysis, electrolysate is dried under the conditions of 80 DEG C after alcohol washes after collecting electrolysis
0.5h obtains graphene powder.
Further, in mixed salt solution, the atomic ratio of Ru:Sn:Co is 4:3:3.Under the special ratios, electrode
The specific capacitance value of material reaches best.
Further, in graphene-metal salt presoma, the content of graphene is 8~12%.Further, graphene
Content be 10%.Under the ratio, metal oxide particle is dispersed in the interlayer of graphene, keeps metal oxide
The synergistic function of high conduction performance, graphene and metal oxide reaches best.
Further, in step S1, the process for the electrolysis that is powered are as follows: power-on voltage be 8~12mV, electric current be 0.02~
0.04A, conduction time are 20~25h.Under the electrolytic condition, it is capable of forming single-layer graphene.
Further, in step S2, solvent is ethanol solution.Further, it is 75%~95% that solvent, which is mass fraction,
Ethanol solution.
In step S3, first graphene is dissolved in the dimethyl formamide solution containing chitosan and acetic acid, then again
It is added in mixed salt solution.Further, the mass ratio of graphene and chitosan is 1:0.2~0.4.Further,
In dimethyl formamide solution, chitosan, acetic acid, dimethylformamide ratio be 0.5g:3g:1L.
Chitosan is a kind of natural polymer for being largely present in nature, has nontoxic, high-intensitive, high adhesive ability etc.
Advantage.A large amount of amino, hydroxyl, acetylamino etc. are contained in chitosan surface, by graphene dispersion in the solution of chitosan-containing, energy
Enough surfaces in graphene form functional membrane, during subsequent graphene and metal ion are compound, enable to metal
Uniform ion is compounded on graphene, forms graphene layer after calcining on an metal oxide.Graphene layer can inhibit metal
The volume deformation of oxide, and metal oxide particle is protected, be conducive to the promotion of electrode material chemical property.
Further, in step S4, in graphene-metal salt presoma calcination process, including with the next stage:
First stage: 230~240 DEG C are warming up to the heating rate of 15~20 DEG C/min, keeps the temperature 10~15min；Second
Stage: 280~300 DEG C are warming up to the heating rate of 2~5 DEG C/min, keeps the temperature 25~40min；Phase III: with 4~6 DEG C/
The rate of temperature fall of min is cooled to 220~230 DEG C, keeps the temperature 10~15min.
First with the heating of faster rate, solvent is quickly removed, and avoids the formation of hole, and then slowly heating, may advantageously facilitate
Form the electrode material of uniform and smooth.Finally, by temperature-fall period, be conducive to the compound of metal oxide and graphene, it can
It effectively avoids electrode material that volume deformation occurs in subsequent charge and discharge process, improves cycle performance.
The present invention also provides ink alkene blended metal oxide electrode materials made from above-mentioned preparation method.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of black alkene blended metal oxide electrode material provided in this embodiment, is made according to following steps:
(1) by the NaCl electrolyte of pairs of graphite electrode insertion 20mg/L, be powered electrolysis, power-on voltage 10mv, electricity
Stream is 0.03A, and conduction time is for 24 hours, after electrolysis, to extract powder alcohol washes and be put into drying box and dry, dry
Temperature is 80 DEG C, dries 0.5h, it is stand-by that collection obtains graphene；
(2) by by Ru:Sn:Co atomic ratio be 4:3:3 by ruthenium trichloride, stannic chloride and cobalt chloride solution in alcohol, obtain
To mixed salt solution；
(3) in mixed salt solution (total amount of metal salt is 60mg), 6mg graphene is added, after mixing, dry
To graphene-metal salt presoma；
(4) graphene-metal salt presoma is kept into 10min at 230 DEG C, is warming up to 280 DEG C of holding 30min, then
It is cooled to 220 DEG C of holding 10min and obtains graphene/metal oxide combination electrode material.
Embodiment 2
A kind of black alkene blended metal oxide electrode material provided in this embodiment, is made according to following steps:
(1) by the NaCl electrolyte of pairs of graphite electrode insertion 20mg/L, be powered electrolysis, power-on voltage 10mv, electricity
Stream is 0.03A, and conduction time is for 24 hours, after electrolysis, to extract powder alcohol washes and be put into drying box and dry, dry
Temperature is 80 DEG C, dries 0.5h, it is stand-by that collection obtains graphene；
(2) ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co,
Obtain mixed salt solution；
(3) in mixed salt solution (total amount of metal salt is 60mg), 6mg graphene is added, after mixing, dry
To graphene-metal salt presoma；
(4) graphene-metal salt presoma is kept into 10min at 230 DEG C, is warming up to 290 DEG C of holding 30min, then
It is cooled to 220 DEG C of holding 10min and obtains graphene/metal oxide combination electrode material.
Embodiment 3
A kind of black alkene blended metal oxide electrode material provided in this embodiment, is made according to following steps:
(1) by the NaCl electrolyte of pairs of graphite electrode insertion 20mg/L, be powered electrolysis, power-on voltage 10mv, electricity
Stream is 0.03A, and conduction time is for 24 hours, after electrolysis, to extract powder alcohol washes and be put into drying box and dry, dry
Temperature is 80 DEG C, dries 0.5h, it is stand-by that collection obtains graphene；
(2) ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co,
Obtain mixed salt solution；
(3) in mixed salt solution (total amount of metal salt is 60mg), 6mg graphene is added, after mixing, dry
To graphene-metal salt presoma；
(4) graphene-metal salt presoma is kept into 10min at 230 DEG C, is warming up to 300 DEG C of holding 30min, then
It is cooled to 220 DEG C of holding 10min and obtains graphene/metal oxide combination electrode material.
Embodiment 4
A kind of black alkene blended metal oxide electrode material provided in this embodiment, is made according to following steps:
(1) by the NaCl electrolyte of pairs of graphite electrode insertion 20mg/L, be powered electrolysis, power-on voltage 10mv, electricity
Stream is 0.03A, and conduction time is for 24 hours, after electrolysis, to extract powder alcohol washes and be put into drying box and dry, dry
Temperature is 80 DEG C, dries 0.5h, it is stand-by that collection obtains graphene；
(2) ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co,
Obtain mixed salt solution；
(3) in mixed salt solution (total amount of metal salt is 60mg), graphene solution is added, it is dry after mixing
Obtain graphene-metal salt presoma, wherein graphene solution are as follows: 6mg graphene is added to containing chitosan (1.5mg) and
In the dimethyl formamide solution of acetic acid；
(4) graphene-metal salt presoma is kept into 10min at 230 DEG C, is warming up to 290 DEG C of holding 30min, then
It is cooled to 220 DEG C of holding 10min and obtains graphene/metal oxide combination electrode material.
Comparative example 1
This comparative example provides a kind of electrode material, is made according to following steps:
Ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co, is obtained
Mixed salt solution；After drying, obtained in 280 DEG C of calcining 30min.
Comparative example 2
This comparative example provides a kind of electrode material, is made according to following steps:
Ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co, is obtained
Mixed salt solution；After drying, obtained in 290 DEG C of calcining 30min.
Comparative example 3
This comparative example provides a kind of electrode material, is made according to following steps:
Ruthenium trichloride, stannic chloride and cobalt chloride will be dissolved in alcohol for 4:3:3 by the atomic ratio of Ru:Sn:Co, is obtained
Mixed salt solution；After drying, obtained in 300 DEG C of calcining 30min.
Comparative example 4
This comparative example provides a kind of graphene, the preparation method comprises the following steps: pairs of graphite electrode is inserted into deionized water, be powered electricity
Solution, power-on voltage 10mv, electric current 0.03A, conduction time are for 24 hours, after electrolysis, to extract powder alcohol washes and put
Enter in drying box and dry, drying temperature is 80 DEG C, dries 0.5h, and collection obtains graphene.
Comparative example 5
This comparative example provides a kind of graphene, the preparation method comprises the following steps: by the NH of pairs of graphite electrode insertion 20mg/L3·H2O electricity
It solves in liquid, be powered electrolysis, power-on voltage 10mv, electric current 0.03A, and conduction time is for 24 hours, after electrolysis, to extract powder
It is dried with alcohol washes and being put into drying box, drying temperature is 80 DEG C, dries 0.5h, and collection obtains graphene.
It is as shown in Figure 1 the shape appearance figure of graphene obtained in the embodiment of the present invention 1, Fig. 2 and Fig. 3 are respectively comparative example 4
With the shape appearance figure of graphene made from comparative example 5.From SEM characterization picture, it can be deduced that draw a conclusion, in the graphene of Fig. 2
Powder particle is more uneven, and has apparent agglomeration in the graphene of Fig. 3.Moreover, this kind of graphene powder particle also compared with
It is uneven.It is found under comparison diagram 2 and Fig. 3, Fig. 1 is the stone for selecting NaCl solution to prepare as electrolyte with electrolysis method
Black alkene is in flakey, and particle is tiny, uniform in size, shape comparison rule.
As shown in figure 4, for the XRD spectrum of electrode material obtained by comparative example 1~3, Fig. 5 show Examples 1 to 3 institute
The XRD spectrum of electrode material obtained.From Fig. 5, it can be clearly seen that 23 ° an apparent peak, this peak nearby occur
It is the characteristic peak of apparent C.
Fig. 6 a is the shape appearance figure of electrode material made from comparative example 1, and Fig. 6 b is the pattern of electrode material made from embodiment 1
Figure, Fig. 6 c are the shape appearance figure of electrode material made from comparative example 2, and Fig. 6 d is the shape appearance figure of electrode material made from embodiment 2, figure
6e is the shape appearance figure of electrode material made from comparative example 3, and Fig. 6 f is the shape appearance figure of electrode material made from embodiment 3.
Fig. 6 a-f belongs to the mud crack shape feature of typical electrode plate.Also, it can be very in Fig. 6 b, Fig. 6 d, Fig. 6 f
Significantly see the covering of graphene.But it is in (Fig. 6 b) that graphene is added at 280 DEG C, it can be seen that electrode surface stone
Black alkene is not uniform enough.At 300 DEG C in (Fig. 6 f), mud crack shape is not obvious enough, therefore is unfavorable for the infiltration of electrolyte, and is scheming
It will also be seen that the covering of graphene is not uniform enough in 6f.And it can be seen that mud crack shape obviously has in (Fig. 6 d) at 290 DEG C
Conducive to the infiltration of electrolyte, and electrode surface uniform and smooth.
The specific capacitance of Examples 1 to 4 and comparative example 1~3 is measured, the results are shown in Table 1.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene blended metal oxide electrode material, which comprises the following steps:
S1 obtains a pair of of graphite electrode and electrolyte, will be inserted into the electrolyte graphite electrode in pairs, and be powered electrolysis,
Obtain the graphene that electrolysis obtains；
Ru salt, Sn salt and Co salt are dissolved in solvent, obtain mixed salt solution, wherein the mixed metal salt is molten by S2
In liquid, the atomic ratio of Ru:Sn:Co is 4:1~4:2~4；
The graphene is added in the mixed salt solution in S3, after mixing, is dried to obtain graphene-metal salt precursor
Body；
The graphene-metal salt presoma is calcined under the conditions of 220 DEG C~300 DEG C, obtains graphene doping metals oxygen by S4
Compound electrode material；
Wherein, in step S4, in the graphene-metal salt presoma calcination process, including with the next stage: the first stage:
230~240 DEG C are warming up to the heating rate of 15~20 DEG C/min, keeps the temperature 10~15min；Second stage: with 2~5 DEG C/min
Heating rate be warming up to 280~300 DEG C, keep the temperature 25~40min；Phase III: cooled down with the rate of temperature fall of 4~6 DEG C/min
To 220~230 DEG C, 10~15min is kept the temperature.
2. preparation method according to claim 1, which is characterized in that in step S1, the electrolyte be concentration be 18~
The NaCl solution of 22mg/L.
3. preparation method according to claim 1, which is characterized in that in the mixed salt solution, Ru:Sn:Co's
Atomic ratio is 4:3:3.
4. preparation method according to claim 1, which is characterized in that in the graphene-metal salt presoma, the stone
The content of black alkene is 8~12wt%.
5. preparation method according to claim 1, which is characterized in that in step S1, the process for the electrolysis that is powered are as follows: be powered electricity
Pressure is 8~12mV, and electric current is 0.02~0.04A, and conduction time is 20~25h.
6. preparation method according to claim 1, which is characterized in that in step S2, the solvent is ethanol solution.
7. preparation method according to claim 1, which is characterized in that in step S3, be first dissolved in the graphene and contain
In the dimethyl formamide solution for having chitosan and acetic acid, it is then then added to the mixed salt solution.
8. preparation method according to claim 7, which is characterized in that the mass ratio of the graphene and the chitosan is
1:0.5~0.8.
9. a kind of graphene blended metal oxide electrode material, which is characterized in that any one institute according to claim 1~8
The preparation method stated is made.
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