CN103833009A - Graphene, its preparation method, electrode slice and supercapacitor - Google Patents
Graphene, its preparation method, electrode slice and supercapacitor Download PDFInfo
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- CN103833009A CN103833009A CN201210480792.8A CN201210480792A CN103833009A CN 103833009 A CN103833009 A CN 103833009A CN 201210480792 A CN201210480792 A CN 201210480792A CN 103833009 A CN103833009 A CN 103833009A
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the electrochemical field, and discloses a graphene, its preparation method, an electrode slice and a supercapacitor. The preparation method of the graphene comprises the following steps: preparing a graphene oxide suspension; preparing a condensed solution containing graphene oxide; preparing a nitrogen doped graphene oxide solution; and preparing the graphene. Graphene obtained through the graphene preparation method has a high specific surface area and a high conductivity, and the adoption of the graphene to the supercapacitor made by adopting grephene has improved energy density and power density; and the method has the advantages of one-step realization of a plurality of performances of the graphene material, operation step simplification, and substantial reduction of the production cost.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to a kind of Graphene and preparation method thereof.The invention still further relates to and use the electrode slice that Graphene is active material, and use the ultracapacitor of this electrode slice.
Background technology
Ultracapacitor (Supercapacitors) claims again electrochemical capacitor (Electrochemical Capacitors) or double layer capacitor (Electric Double Layer Capacitors), it is a kind of novel energy-storing element between traditional capacitor and battery, there is more high-specific capacitance super and energy density compared with traditional capacitor, there is higher power density compared with battery; Because ultracapacitor has that the speed of discharging and recharging is fast, environmentally safe and the advantage such as have extended cycle life, promise to be novel green energy resource in this century.Electrode materials is the important component part of ultracapacitor, be affect ultracapacitor capacitive character can and the key factor of production cost, therefore research and develop high-performance, electrode materials is the important content of ultracapacitor research work cheaply.The electrode materials of the ultracapacitor of research mainly contains Carbon Materials, metal oxide and hydrate electrode materials thereof and conductive polymer electrodes material at present.
At present the electrode materials of double electric layers supercapacitor is mainly carbon material, has good heat conduction and conductivity, higher specific surface area, is widely used in electrochemical field and makes electrode materials, and carbon material is the most successfully one of electrode materials of current industrialization.At present, the research of carbon-based electrode material mainly concentrates on research and development and has the research of the aspects such as porous carbon materials that high-specific surface area, internal resistance are less.Graphene has high specific surface area, fabulous electroconductibility, good thermal conductivity, and the cost performance of the Graphene obtaining by graphite oxide reduction method is higher, and good stability, is the ideal electrode material of ultracapacitor.The ultracapacitor that use Graphene produces will be all higher than the energy storage density of at present all ultracapacitors.But the actual Graphene electrodes material preparing is due to reasons such as reunions, and capacity is on the low side, and in water system, capacity is 135F/g, organic system capacity 99F/g, Distance Theory capacity (550F/g) differs far away.
Summary of the invention
Based on the problems referred to above, problem to be solved by this invention is to provide the preparation method of a kind of specific conductivity, electrical capacity is high and energy storage density is higher Graphene.
Technical scheme of the present invention is as follows:
A preparation method for Graphene, comprises the steps:
By the graphite oxide ultrasonic dispersion treatment that is added to the water, obtaining concentration is the graphene oxide suspension of 1～20mg/ml;
The KOH solution that is 1～500g/L by concentration joins in described graphene oxide suspension, stirs, and obtains condensing shape solution;
The NaOH solution that is 1～500g/L by concentration joins in described cohesion shape solution, fully stirs 1～5h, obtains mixing solutions;
The above-mentioned mixing solutions that obtains is filtered, and screening is carried out to drying treatment, more dried screening is put into retort furnace and under inert atmosphere, carry out high-temperature calcination, cooling after, washing, filter, dry, obtain described Graphene.
Preferably, the preparation method of described Graphene, wherein, the described ultrasonic dispersion treatment time is 1～5h.
Preferably, the preparation method of described Graphene, wherein, in described cohesion shape solution, the mass ratio of KOH and graphene oxide is 1～30: 1.
Preferably, the preparation method of described Graphene, wherein, in described mixing solutions, the mass ratio of NaOH and graphene oxide is 1～10: 1.
Preferably, the preparation method of described Graphene, wherein, in described drying treatment process, drying treatment temperature is 60～80 DEG C, the drying treatment time is 24～48h.
Preferably, the preparation method of described Graphene, wherein, when described high-temperature calcination, temperature is 800～1200 DEG C, calcination time is 1～5h.
The present invention also provides a kind of Graphene, and this Graphene adopts above-mentioned preparation method to make.
The present invention also provides a kind of electrode slice, comprises collector, and is coated in the active material of described collection liquid surface; This active material comprises the above-mentioned Graphene making, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor; The mass ratio of described Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor is 88: 10: 2.
The present invention also provides a kind of ultracapacitor, and its electrode adopts above-mentioned electrode slice.
The preparation method of Graphene provided by the invention, KOH can be good at activating Graphene, obtains the grapheme material 1500～3000m of high-specific surface area
2/ g, the Graphene of high-specific surface area can have been given play to higher capacity; In KOH, adding NaOH to carry out common activation can increase the density of the rear Graphene of activation, thereby increases the volumetric capacitance of Graphene.This is because the activity of K is better than Na, and KOH can penetrate into more in graphene sheet layer structure and activate.Reach 750 DEG C of left and right in temperature of reaction, K (762 DEG C of boiling points) separates out, and the steam of K is constantly squeezed in the structure of Graphene carbon atomic layer is expanded, and forms more tiny hole, promptly increases the specific surface area of porous charcoal.And the boiling point of Na higher (883 DEG C), more difficult formation steam, is molten state, poor fluidity, and seepage velocity is slower.NaOH activation is mainly taking the corrasion of NaOH as main, and its activation forms more mesopores, and pore volume is not as KOH activation porous charcoal, make tap density taking micropore as main KOH high.
Brief description of the drawings
Fig. 1 is preparation technology's schema of Graphene of the present invention.
Embodiment
The preparation method of Graphene provided by the invention, as shown in Figure 1, its process flow steps is as follows:
S1, by the graphite oxide ultrasonic dispersion 1～5h that is added to the water, obtaining concentration is the graphene oxide suspension of 1～20mg/ml;
S2, the KOH solution that is 1～500g/L by concentration join in above-mentioned functionalized graphene suspension, stir until appearance cohesion obtains condensing shape solution; Wherein, in cohesion shape solution, the mass ratio of KOH and graphene oxide is 1～30: 1;
S3, the NaOH solution that is 1～500g/L by concentration join in cohesion shape solution, fully stir 1～5h, obtain mixing solutions; Wherein, in mixing solutions, the mass ratio of NaOH and graphene oxide is 1～10: 1;
S4, the mixing solutions that step S3 is obtained filter, screening is placed in 60～80 DEG C of drying treatment 24～48h, again dried screening is put into retort furnace, and under inert atmosphere (atmosphere of the gas mixture composition of nitrogen, argon gas or nitrogen and argon gas), in 800～1200 DEG C high-temperature calcination 1～5h, cooling after, washing, filter, the dry Graphene that obtains.
The preparation method of Graphene provided by the invention, KOH can be good at activating Graphene, obtains the grapheme material 1500～3000m of high-specific surface area
2/ g, the Graphene of high-specific surface area can have been given play to higher capacity; In KOH, adding NaOH to carry out common activation can increase the density of the rear Graphene of activation, thereby increases the volumetric capacitance of Graphene.This is because the activity of K is better than Na, and KOH can penetrate into more in graphene sheet layer structure and activate.Reach 750 DEG C of left and right in temperature of reaction, K (762 DEG C of boiling points) separates out, and the steam of K is constantly squeezed in the structure of Graphene carbon atomic layer is expanded, and forms more tiny hole, promptly increases the specific surface area of porous charcoal.And the boiling point of Na higher (883 DEG C), more difficult formation steam, is molten state, poor fluidity, and seepage velocity is slower.NaOH activation is mainly taking the corrasion of NaOH as main, and its activation forms more mesopores, and pore volume is not as KOH activation porous charcoal, make tap density taking micropore as main KOH high.
Below the making method of ultracapacitor:
1, prepare electrode slice
First, the ratio that is 88: 10: 2 according to mass ratio, selects the above-mentioned Graphene making, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor to mix, and obtains gel slurry;
Secondly, by gel slurry be coated in collector (as, aluminium foil, nickel foil, nickel screen, Copper Foil, preferably aluminium foil) upper, drying, roll film, trimming processing, make electrode slice.
2, prepare ultracapacitor
Select two of the above-mentioned electrode slices making, respectively as positive plate and negative plate; Order stack of laminations according to positive plate, barrier film, negative plate is dressed up battery core, then uses battery housing seal battery core, injects electrolytic solution subsequently by the spout being arranged on battery container in battery container, and sealing spout, obtains ultracapacitor;
Wherein, electrolytic solution adopts BMIMBF
4, EMIMTFSI plasma liquid, also can adopt conventional electrolytic solution TEABF
4/ AN.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1～4th, the preparation method of Graphene.
Embodiment 1
(1) 1g graphite oxide is added to the water ultrasonic dispersion 1h, obtains forming the graphene oxide suspension of concentration 1mg/ml,
(2) the KOH solution that compound concentration is 1g/L, joins KOH solution in above-mentioned graphene oxide suspension, stirs until appearance cohesion obtains condensing shape solution; Wherein, in cohesion shape solution, the mass ratio of KOH and graphene oxide is 1: 1;
(3) the NaOH solution that compound concentration is 1g/L, joins NaOH solution in above-mentioned cohesion shape solution, fully stirs 1h, obtains mixing solutions; Wherein, in mixing solutions, the mass ratio of NaOH and graphene oxide is 1: 1;
(4) mixing solutions obtained above is filtered, screening is in 60 DEG C of dry 48h, more dried screening is put into retort furnace, the lower 800 DEG C of high-temperature calcinations reaction of nitrogen atmosphere 5h, cooling after, washing, filter, the dry Graphene that obtains.
Embodiment 2
(1) 20g graphite oxide is added to the water ultrasonic dispersion 5h, obtaining concentration is the graphene oxide suspension of 20mg/ml,
(2) the KOH solution that compound concentration is 500g/L, joins KOH solution in above-mentioned mixing solutions, stirs until appearance cohesion shape solution wherein, condenses in shape solution, and the mass ratio of KOH and Graphene is 30: 1;
(3) the NaOH solution that compound concentration is 500g/L, joins NaOH solution in above-mentioned cohesion shape solution, fully stirs 5h, obtains mixing solutions; Wherein, in mixing solutions, the mass ratio of NaOH and graphene oxide is 3: 1;
(4) mixing solutions obtained above is filtered, screening is in 80 DEG C of dry 24h, more dried screening is put into retort furnace, and in the lower 1200 DEG C of high-temperature calcinations reaction of argon atmosphere 1h, cooling after, washing, filter, the dry Graphene that obtains.
Embodiment 3
(1) 10g graphite oxide is added to the water ultrasonic dispersion 2h, obtaining concentration is the graphene oxide suspension of 10mg/ml;
(2) the KOH solution that compound concentration is 100g/L, joins KOH solution in above-mentioned graphene oxide suspension, stirs until appearance cohesion shape solution wherein, condenses in shape solution, and the mass ratio of KOH and Graphene is 10: 1;
(3) the NaOH solution that compound concentration is 100g/L, joins NaOH solution in upper cohesion shape solution, fully stirs 2h, obtains mixing solutions; Wherein, in mixing solutions, the mass ratio of NaOH and graphene oxide is 5: 1;
(4) mixing solutions obtained above is filtered, screening is in 70 DEG C of dry 36h, again dried screening is put into retort furnace, and nitrogen and the lower 900 DEG C of high-temperature calcinations reaction of argon gas gas mixture atmosphere 4h, cooling after, washing, filter, the dry Graphene that obtains.
Embodiment 4
(1) 5g graphite oxide is added to the water ultrasonic dispersion 3h, obtaining concentration is the graphene oxide suspension of 5mg/ml;
(2) the KOH solution that compound concentration is 300g/L, joins KOH solution in above-mentioned graphene oxide suspension, stirs until there is cohesion shape solution; Wherein, now condense in shape solution, the mass ratio of KOH and Graphene is 20: 1;
(3) the NaOH solution that compound concentration is 300g/L, joins above-mentioned now cohesion in shape solution by NaOH solution, fully stirs 3h, obtains mixing solutions; Wherein, in mixing solutions, the mass ratio of NaOH and graphene oxide is 10: 1;
(4) mixing solutions obtained above is filtered, screening is in 75 DEG C of dry 30h, more dried screening is put into retort furnace, and the lower 1000 DEG C of high-temperature calcinations reaction of nitrogen atmosphere 3h, cooling after, washing, filter, the dry Graphene that obtains.
The density of the Graphene to embodiment 1～4 preparation is tested, and result is as shown in table 1:
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| The density g/cm of Graphene 3 | 0.52 | 0.47 | 0.48 | 0.50 |
Embodiment 5～8th, the Graphene of preparing using embodiment 1～4 is respectively as the application of the active material of super capacitor electrode slice.
Embodiment 5
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 1 active material as electrode slice;
Secondly, the ratio that is 88: 10: 2 according to mass ratio, Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Get above-mentioned two plate electrode sheets, respectively as positive, negative electrode plate, dress up battery core according to the order stack of laminations of pole piece, barrier film, negative plate, then use battery housing seal battery core, in battery container, inject BMIMBF by the spout being arranged on battery container subsequently
4il electrolyte, sealing spout, obtains ultracapacitor.
Embodiment 6
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 2 active material as electrode slice;
Secondly, the ratio that is 88: 10: 2 according to mass ratio, Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Get above-mentioned two plate electrode sheets, respectively as positive, negative electrode plate, order stack of laminations according to pole piece, barrier film, negative plate is dressed up battery core, use again battery housing seal battery core, in battery container, inject EMIMTFSI il electrolyte by the spout being arranged on battery container subsequently, sealing spout, obtains ultracapacitor.
Embodiment 7
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 3 active material as electrode slice;
Secondly, the ratio that is 88: 10: 2 according to mass ratio, Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Get above-mentioned two plate electrode sheets, respectively as positive, negative electrode plate, dress up battery core according to the order stack of laminations of pole piece, barrier film, negative plate, then use battery housing seal battery core, in battery container, inject TEABF by the spout being arranged on battery container subsequently
4/ AN electrolytic solution, sealing spout, obtains ultracapacitor.
Embodiment 8
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 4 active material as electrode slice;
Secondly, the ratio that is 88: 10: 2 according to mass ratio, Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Get above-mentioned two plate electrode sheets, respectively as positive, negative electrode plate, dress up battery core according to the order stack of laminations of pole piece, barrier film, negative plate, then use battery housing seal battery core, in battery container, inject TEABF by the spout being arranged on battery container subsequently
4/ AN electrolytic solution, sealing spout, obtains ultracapacitor.
The charge-discharge test volumetric capacitance result that embodiment 5～8 is made to ultracapacitor is as shown in table 2:
Table 2
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Volume and capacity ratio F/cm 3 | 75 | 68 | 71 | 73 |
The Graphene capacity activating with KOH is separately at 60F/cm
3left and right; As shown in Table 2, the Graphene volumetric capacitance amount that prepared by the present invention exceedes 68F/cm
3, capacity has had large increase.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
By the graphite oxide ultrasonic dispersion treatment that is added to the water, obtaining concentration is the graphene oxide suspension of 1～20mg/ml;
The KOH solution that is 1～500g/L by concentration joins in described graphene oxide suspension, stirs, and obtains condensing shape solution;
The NaOH solution that is 1～500g/L by concentration joins in described cohesion shape solution, fully stirs 1～5h, obtains mixing solutions;
The above-mentioned mixing solutions that obtains is filtered, and screening is carried out to drying treatment, more dried screening is put into retort furnace and under inert atmosphere, carry out high-temperature calcination, cooling after, washing, filter, dry, obtain described Graphene.
2. the preparation method of Graphene according to claim 1, is characterized in that, the described ultrasonic dispersion treatment time is 1～5h.
3. the preparation method of Graphene according to claim 1, is characterized in that, in described cohesion shape solution, the mass ratio of KOH and graphene oxide is 1～30: 1.
4. the preparation method of Graphene according to claim 1, is characterized in that, in described mixing solutions, the mass ratio of NaOH and graphene oxide is 1～10: 1.
5. the preparation method of Graphene according to claim 1, is characterized in that, in described drying treatment process, drying treatment temperature is 60～80 DEG C, and the drying treatment time is 24～48h.
6. the preparation method of Graphene according to claim 1, is characterized in that, when described high-temperature calcination, temperature is 800～1200 DEG C, and calcination time is 1～5h.
7. a Graphene, is characterized in that, this Graphene adopts the arbitrary described preparation method of claim 1～6 to make.
8. an electrode slice, comprises collector, and is coated in the active material of described collection liquid surface; It is characterized in that, described active material comprises Graphene claimed in claim 7, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor; The mass ratio of described Graphene, polyvinylidene difluoride (PVDF) binding agent and acetylene black conductor is 88: 10: 2.
9. a ultracapacitor, is characterized in that, comprises electrode slice claimed in claim 8.
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