CN103839691A - Nitrogen-doped graphene composite material, preparation method thereof, electrode plate and supercapacitor - Google Patents
Nitrogen-doped graphene composite material, preparation method thereof, electrode plate and supercapacitor Download PDFInfo
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- CN103839691A CN103839691A CN201210484414.7A CN201210484414A CN103839691A CN 103839691 A CN103839691 A CN 103839691A CN 201210484414 A CN201210484414 A CN 201210484414A CN 103839691 A CN103839691 A CN 103839691A
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Abstract
The invention pertains to the field of electrochemistry, and discloses a nitrogen-doped graphene composite material, a preparation method thereof, an electrode plate and a supercapacitor. The preparation method of the nitrogen-doped graphene composite material comprises the following steps: oxidized graphene soliquoid is prepared; a condensed solution containing oxidized graphene is prepared; a nitrogen-doped oxidized graphene solution is prepared; and the nitrogen-doped graphene composite material is prepared. According to the nitrogen-doped graphene composite material preparation method of the invention, the nitrogen-doped graphene composite material having advantages of high specific surface area and high electrical conductivity can be obtained, by adopting the nitrogen-doped graphene composite material to prepare the supercapacitor, the energy density and power density of the capacitor can be improved; and according to the method, various performances of the grapheme material can be realized in one step, the operating step can be simplified, and the production cost can be greatly reduced.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to a kind of nitrogen-doped graphene composite material and preparation method thereof.The invention still further relates to and use the electrode slice that nitrogen-doped graphene composite material is active material, and use the ultracapacitor of this electrode slice.
Background technology
Ultracapacitor (Supercapacitors) claims again electrochemical capacitor (Electrochemical Capacitors) or double electric 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 material 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 material is the important content of ultracapacitor research work cheaply.The electrode material of the ultracapacitor of research mainly contains Carbon Materials, metal oxide and hydrate electrode material thereof and conductive polymer electrodes material at present.
At present the electrode material of double electric layers supercapacitor is mainly material with carbon element, has good heat conduction and electric conductivity, higher specific area, is widely used in electrochemical field and makes electrode material, and material with carbon element is the most successfully one of electrode material 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 area, fabulous conductivity, good thermal conductivity, and the cost performance of the Graphene obtaining by graphite oxide reducing process 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 conductivity, capacitance is high and energy storage density is higher nitrogen-doped graphene composite material.
Technical scheme of the present invention is as follows:
A preparation method for nitrogen-doped graphene composite material, 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 urea, ammonium carbonate, carbonic hydroammonium or the ammonium oxalate solution that are 1 ~ 100g/L by concentration join in described cohesion shape solution, fully stir 1 ~ 5h, obtain nitrogen doped with oxygen functionalized graphene precursor solution;
By the above-mentioned nitrogen doped with oxygen functionalized graphene precursor solution filter that obtains, and screening is dried to processing, again dried screening put into Muffle furnace and under inert atmosphere, carried out high-temperature calcination, cooling after, washing, filter, dry, obtain described nitrogen-doped graphene composite material.
Preferably, the preparation method of described nitrogen-doped graphene composite material, wherein, the described ultrasonic dispersion treatment time is 1 ~ 5h.
Preferably, the preparation method of described nitrogen-doped graphene composite material, wherein, in described cohesion shape solution, the mass ratio of KOH and graphene oxide is 1 ~ 30:1.
Preferably, the preparation method of described nitrogen-doped graphene composite material, wherein, in described nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of urea, ammonium carbonate, carbonic hydroammonium or ammonium oxalate and graphene oxide is 1 ~ 10:1.
Preferably, the preparation method of described nitrogen-doped graphene composite material, wherein, in described dry processing procedure, dry treatment temperature is 60 ~ 80 ℃, the dry processing time is 24 ~ 48h.
Preferably, the preparation method of described nitrogen-doped graphene composite material, wherein, when described high-temperature calcination, temperature is 800 ~ 1200 ℃, calcination time is 1 ~ 5h.
The present invention also provides a kind of nitrogen-doped graphene composite material, and this nitrogen-doped graphene composite material by adopting is above-mentioned preparation method 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 nitrogen-doped graphene composite material making, Kynoar binding agent and acetylene black conductor; The mass ratio of described nitrogen-doped graphene composite material, Kynoar 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 nitrogen-doped graphene composite material 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; Adopt the labile urea of high temperature to react with graphite oxide, the condition urea of high temperature can resolve into ammonia can provide the nitrogenous source of doping to Graphene, makes Graphene generate nitrogen-doped graphene composite material; At the temperature of 800 ~ 1200 ℃, reduction can be that surface oxygen functional group on Graphene reduces fully, residual less functional group on Graphene.In hot environment under the protection of inert gas, there are three kinds of reactions, 1, graphite oxide is reduced to Graphene simultaneously; 2, KOH activation Graphene, forms high-specific surface area; 3, urea decomposition becomes ammonia to adulterate to Graphene, obtains nitrogen-doped graphene composite material, and three reactions realize and settling at one go, have simplified operating procedure, greatly reduce production cost.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of nitrogen-doped graphene composite material of the present invention.
Embodiment
The preparation method of nitrogen-doped graphene composite material 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 urea, ammonium carbonate, carbonic hydroammonium or the ammonium oxalate solution that are 1 ~ 100g/L by concentration join in cohesion shape solution, fully stir 1 ~ 5h, obtain nitrogen doped with oxygen functionalized graphene precursor solution; Wherein, in nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of urea, ammonium carbonate, carbonic hydroammonium or ammonium oxalate and graphene oxide is 1 ~ 10:1;
S4, the nitrogen doped with oxygen functionalized graphene precursor solution filter that step S3 is obtained, screening is placed in 60 ~ 80 ℃ of dry 24 ~ 48h of processing, again dried screening is put into Muffle furnace, and under inert atmosphere (atmosphere of the gaseous mixture composition of nitrogen, argon gas or nitrogen and argon gas), in 800 ~ 1200 ℃ high-temperature calcination 1 ~ 5h, cooling after, washing, filter, the dry nitrogen-doped graphene composite material that obtains.
The preparation method of nitrogen-doped graphene composite material 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; Adopt the labile urea of high temperature to react with graphite oxide, condition urea, the ammonium carbonate etc. of high temperature can resolve into ammonia can provide the nitrogenous source of doping to Graphene, makes Graphene generate nitrogen-doped graphene composite material; At the temperature of 800 ~ 1200 ℃, reduction can be that surface oxygen functional group on Graphene reduces fully, residual less functional group on Graphene.In hot environment under the protection of inert gas, there are three kinds of reactions, 1, graphite oxide is reduced to Graphene simultaneously; 2, KOH activation Graphene, forms high-specific surface area; 3, urea decomposition becomes ammonia to adulterate to Graphene, obtains nitrogen-doped graphene composite material, and three reactions realize and settling at one go, have simplified operating procedure, greatly reduce production cost.
Below the manufacture method of ultracapacitor:
1, prepare electrode slice
First, the ratio that is 88:10:2 according to mass ratio, selects the above-mentioned nitrogen-doped graphene composite material making, Kynoar 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 electrolyte subsequently by the liquid injection port being arranged on battery container in battery container, and sealing liquid injection port, obtains ultracapacitor;
Wherein, electrolyte adopts BMIMBF
4, EMIMTFSI plasma liquid, also can adopt conventional electrolyte 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 nitrogen-doped graphene composite material.
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) urea liquid that compound concentration is 1g/L, joins urea liquid in above-mentioned cohesion shape solution, fully stirs 1h, obtains nitrogen doped with oxygen functionalized graphene precursor solution; Wherein, in nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of urea and graphene oxide is 1:1;
(4) nitrogen doped with oxygen functionalized graphene precursor solution obtained above is filtered, screening is in 60 ℃ of dry 48h, again dried screening is put into Muffle furnace, the lower 800 ℃ of high-temperature calcinations reaction of nitrogen atmosphere 5h, cooling after, washing, filter, the dry nitrogen-doped graphene composite material 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 dispersion liquid, stirs until appearance cohesion shape solution wherein, condenses in shape solution, and the mass ratio of KOH and Graphene is 30:1;
(3) sal volatile that compound concentration is 100g/L, joins sal volatile in above-mentioned cohesion shape solution, fully stirs 5h, obtains nitrogen doped with oxygen functionalized graphene precursor solution; Wherein, in nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of ammonium carbonate and graphene oxide is 10:1;
(4) nitrogen doped with oxygen functionalized graphene precursor solution obtained above is filtered, screening is in 80 ℃ of dry 24h, again dried screening is put into Muffle furnace, and in the lower 1200 ℃ of high-temperature calcinations reaction of argon atmosphere 1h, cooling after, washing, filter, the dry nitrogen-doped graphene composite material 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) ammonium bicarbonate soln that compound concentration is 20g/L, joins ammonium bicarbonate soln in upper cohesion shape solution, fully stirs 2h, obtains nitrogen doped with oxygen functionalized graphene solution; Wherein, in nitrogen doped with oxygen functionalized graphene solution, the mass ratio of carbonic hydroammonium and graphene oxide is 5:1;
(4) nitrogen doped with oxygen functionalized graphene solution obtained above is filtered, screening is in 70 ℃ of dry 36h, again dried screening is put into Muffle furnace, and nitrogen and the lower 900 ℃ of high-temperature calcinations reaction of argon gas gaseous mixture atmosphere 4h, cooling after, washing, filter, the dry nitrogen-doped graphene composite material 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) ammonium oxalate solution that compound concentration is 70g/L, joins above-mentioned now cohesion in shape solution by ammonium oxalate solution, fully stirs 3h, obtains nitrogen doped with oxygen functionalized graphene precursor solution; Wherein, in nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of ammonium oxalate and graphene oxide is 7:1;
(4) nitrogen doped with oxygen functionalized graphene precursor solution obtained above is filtered, screening is in 75 ℃ of dry 30h, again dried screening is put into Muffle furnace, and the lower 1000 ℃ of high-temperature calcinations reaction of nitrogen atmosphere 3h, cooling after, washing, filter, the dry nitrogen-doped graphene composite material that obtains.
The nitrogen-doped graphene material of embodiment 1 ~ 4 preparation is tested to the specific area obtaining by BET as shown in table 1:
Table 1
| Embodiment | 1 | 2 | 3 | 4 |
| The specific area m of nitrogen-doped graphene composite material 2/g | 2208 | 3102 | 2508 | 2835 |
Graphene specific area prepared by conventional thermal reduction method is ~ 900m
2/ g, as shown in Table 1, the present invention obtains nitrogen-doped graphene composite material specific area and has substantially exceeded conventional method.
The conductivity value that the nitrogen-doped graphene composite material of embodiment 1 ~ 4 preparation is obtained by four point probe tester, as shown in table 2:
Table 2
| Embodiment | 1 | 2 | 3 | 4 |
| The conductivity s/m of nitrogen-doped graphene composite material | 1200 | 2100 | 1700 | 1800 |
Graphene conductivity 150-240S/m prepared by conventional thermal reduction method; As shown in Table 2, the nitrogen-doped graphene composite material that prepared by the present invention has obtained higher conductivity.
Embodiment 5 ~ 8th, the nitrogen-doped graphene composite material 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 nitrogen-doped graphene composite material prepared by embodiment 1 active material as electrode slice;
Secondly, the ratio that is 88:10:2 according to mass ratio, nitrogen-doped graphene composite material, Kynoar 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 BMIMBF4 il electrolyte by the liquid injection port being arranged on battery container subsequently, sealing liquid injection port, obtains ultracapacitor.
Embodiment 6
1, prepare super capacitor electrode slice
First, select nitrogen-doped graphene composite material prepared by embodiment 2 active material as electrode slice;
Secondly, the ratio that is 88:10:2 according to mass ratio, nitrogen-doped graphene composite material, Kynoar 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 liquid injection port being arranged on battery container subsequently, sealing liquid injection port, obtains ultracapacitor.
Embodiment 7
1, prepare super capacitor electrode slice
First, select nitrogen-doped graphene composite material prepared by embodiment 3 active material as electrode slice;
Secondly, the ratio that is 88:10:2 according to mass ratio, nitrogen-doped graphene composite material, Kynoar 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 liquid injection port being arranged on battery container subsequently
4/ AN electrolyte, sealing liquid injection port, obtains ultracapacitor.
Embodiment 8
1, prepare super capacitor electrode slice
First, select nitrogen-doped graphene composite material prepared by embodiment 4 active material as electrode slice;
Secondly, the ratio that is 88:10:2 according to mass ratio, nitrogen-doped graphene composite material, Kynoar 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 liquid injection port being arranged on battery container subsequently
4/ AN electrolyte, sealing liquid injection port, obtains ultracapacitor.
The charge-discharge test result that embodiment 5 ~ 8 is made to ultracapacitor is as shown in table 3:
Table 3
| Embodiment | 5 | 6 | 7 | 8 |
| Specific capacity F/g | 198 | 234 | 226 | 228 |
Nitrogen-doped graphene composite material capacity prepared by thermal reduction method is at 100F/g, and the nitrogen-doped graphene composite material capacity activating with KOH is separately in 150F/g left and right; As shown in Table 3, nitrogen-doped graphene composite material capacity prepared by the present invention exceedes 200F/g, and 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 nitrogen-doped graphene composite material, 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 urea, ammonium carbonate, carbonic hydroammonium or the ammonium oxalate solution that are 1 ~ 100g/L by concentration join in described cohesion shape solution, fully stir 1 ~ 5h, obtain nitrogen doped with oxygen functionalized graphene precursor solution;
By the above-mentioned nitrogen doped with oxygen functionalized graphene precursor solution filter that obtains, and screening is dried to processing, again dried screening put into Muffle furnace and under inert atmosphere, carried out high-temperature calcination, cooling after, washing, filter, dry, obtain described nitrogen-doped graphene composite material.
2. the preparation method of nitrogen-doped graphene composite material according to claim 1, is characterized in that, the described ultrasonic dispersion treatment time is 1 ~ 5h.
3. the preparation method of nitrogen-doped graphene composite material 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 nitrogen-doped graphene composite material according to claim 1, is characterized in that, in described nitrogen doped with oxygen functionalized graphene precursor solution, the mass ratio of urea, ammonium carbonate, carbonic hydroammonium or ammonium oxalate and graphene oxide is 1 ~ 10:1.
5. the preparation method of nitrogen-doped graphene composite material according to claim 1, is characterized in that, in described dry processing procedure, dry treatment temperature is 60 ~ 80 ℃, and the dry processing time is 24 ~ 48h.
6. the preparation method of nitrogen-doped graphene composite material according to claim 1, is characterized in that, when described high-temperature calcination, temperature is 800 ~ 1200 ℃, and calcination time is 1 ~ 5h.
7. a nitrogen-doped graphene composite material, is characterized in that, this nitrogen-doped graphene composite material by adopting claim 1 ~ 6 is arbitrary described preparation method 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 nitrogen-doped graphene composite material claimed in claim 7, Kynoar binding agent and acetylene black conductor; The mass ratio of described nitrogen-doped graphene composite material, Kynoar 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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| CN105140050A (en) * | 2015-08-20 | 2015-12-09 | 西安岳达植物科技有限公司 | Preparation method for nitrogen sulfur doped wormlike graphite supercapacitor electrode material |
| CN105374572A (en) * | 2015-12-16 | 2016-03-02 | 天津工业大学 | Low cost high specific energy long-acting capacitor electrode material and preparation method for the same |
| CN114864302A (en) * | 2022-05-09 | 2022-08-05 | 晋江瑞碧科技有限公司 | Preparation method of nitrogen-doped graphene oxide-based flexible supercapacitor |
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| CN102070140A (en) * | 2011-02-28 | 2011-05-25 | 无锡第六元素高科技发展有限公司 | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment |
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| CN104851604A (en) * | 2015-04-02 | 2015-08-19 | 安徽江威精密制造有限公司 | Electrode material prepared by use of waste PVC and used for supercapacitor and preparation method |
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| CN105374572A (en) * | 2015-12-16 | 2016-03-02 | 天津工业大学 | Low cost high specific energy long-acting capacitor electrode material and preparation method for the same |
| CN114864302A (en) * | 2022-05-09 | 2022-08-05 | 晋江瑞碧科技有限公司 | Preparation method of nitrogen-doped graphene oxide-based flexible supercapacitor |
| CN114864302B (en) * | 2022-05-09 | 2023-08-18 | 武夷学院 | Preparation method of nitrogen-doped graphene oxide based flexible supercapacitor |
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