CN109003826A - N and S codope graphene-graphene nanobelt aeroge preparation method - Google Patents
N and S codope graphene-graphene nanobelt aeroge preparation method Download PDFInfo
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- CN109003826A CN109003826A CN201810841851.7A CN201810841851A CN109003826A CN 109003826 A CN109003826 A CN 109003826A CN 201810841851 A CN201810841851 A CN 201810841851A CN 109003826 A CN109003826 A CN 109003826A
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- C01B32/15—Nano-sized carbon materials
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
The invention discloses a kind of preparation methods of N and S codope graphene-graphene nanobelt aeroge, belong to electrode material preparation technical field.After first mixing stannic oxide/graphene nano band and graphene oxide, deionized water is added, obtains mixed liquor after ultrasound is uniform；Pyrroles and thiophene are added into mixed liquor, carries out a hydro-thermal reaction, obtains hydrogel；Obtained hydrogel is put into KNO3In solution, secondary hydro-thermal reaction is carried out, after being cooled to room temperature, using filter, washing and freeze-drying；Products therefrom thermal cracking in argon atmosphere after being freeze-dried, is made N the and S codope graphene-graphene nanobelt aeroge.Present invention N and S in graphene aerogel, wherein the codope of N and S can further enhance the reactivity and electric conductivity of carbon material, compared to single N or S dopant material, by introducing more active sites, to improve its chemical property, it is expected in the electrode material applied to supercapacitor.
Description
Technical field
The invention belongs to electrode material preparation technical fields, and in particular to a kind of N and S codope graphene-graphene is received
Preparation method of the rice with aeroge.
Background technique
In all carbon materials, as carbon nanotube, nanofiber, porous carbon, hollow nano-sphere, carbon paste capsule, graphene are received
Rice piece, graphene nanobelt and its composite material, graphene are better than other carbon materials due to its outstanding electronics and mechanical performance
Material.Although graphene has been achieved for sizable progress in supercapacitor, performance is still barely satisfactory.This is because
Strong Van der Waals force and the interaction of π-π lamination between graphene layer form graphite-like structure so that they are easy aggregation, thus
The loss for leading to effective ratio area reduces its specific capacitance.Therefore, in order to make full use of the chemical property of graphene, it is necessary to
Effectively inhibit it from stack-up issue.
Graphene aerogel represents a kind of novel globality carbonaceous material, flourishing hole, ultralow density with
And excellent conductive characteristic imparts graphene aerogel before the wide application in the fields such as the energy, environmental protection and catalysis
Scape is research hotspot in recent years.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, providing a kind of N and S codope graphene-graphene nano
Preparation method with aeroge.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of N and S codope graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) after mixing graphene oxide made from stannic oxide/graphene nano band made from step (1) and step (2), addition is gone
Ionized water obtains the mixed liquor that concentration is 2 mg/mL after ultrasound is uniform；
(4) pyrroles and thiophene are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction, reaction temperature is 165 ~
180 DEG C, the reaction time is 3 ~ 5 h, obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2 M3In solution, secondary hydro-thermal reaction is carried out, reaction temperature is
120 ~ 130 DEG C, the reaction time is 2 ~ 3 h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) it by products therefrom 2 h of thermal cracking at 1050 ~ 1100 DEG C in argon atmosphere after step (5) freeze-drying, is made
N the and S codope graphene-graphene nanobelt aeroge.
The mass ratio of stannic oxide/graphene nano band described in step (3) and graphene oxide is 1:1.
The mass ratio of pyrroles described in step (4) and thiophene is 1:1, and wherein the additional amount of pyrroles is graphene oxide
1wt%。
N and S codope graphene-graphene nanobelt aeroge obtained is used in electrode material, specific steps are as follows:
By N and S codope graphene-graphene nanobelt aeroge, acetylene black, ptfe emulsion according to mass ratio be 90:5:5
Ratio be added in same weighing bottle, be uniformly mixed and sample be blown to paste with hair dryer, using nickel foam as collector,
Pastes is coated in nickel foam, is dried in vacuo at 120 DEG C for 24 hours, it is final that required electrode is made.
The beneficial effects of the present invention are:
(1) present invention is inserted into graphene nanobelt between graphene synusia, helps to improve the electric conductivity of graphene layer, and
Carbon nanotube can be used as spacer also to prevent the aggregation of graphene layer；In addition, low-dimensional carbon material is self-assembled into three-dimensional porous receive
Rice structural network, can greatly improve its specific surface area, big electrode/electrolyte contact area is provided for charge transfer reaction,
Shorten ion transport length, to improve chemical property；
(2) present invention N and S in graphene aerogel, wherein the codope of N and S can further enhance the reaction of carbon material
Property and electric conductivity, compared to single N or S dopant material, by introducing more active sites, to improve its electrochemistry
Energy.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
The preparation of stannic oxide/graphene nano band:
(A) in the dense H of 36 mL2SO44 mL are added after 2 h of magnetic agitation in 0.15 g multi-walled carbon nanotube (MWCNTs) of middle addition
H3PO4, continue to stir 15 min；1.2 g KMnO are added4Afterwards, 2 h of heating stirring in 65 DEG C of oil baths is moved to.It is cold to the end of reacting
But to after room temperature, 100 mL ice water (30% H containing 5 mL is added2O2), stand 14 h；
(B) supernatant liquor is removed after the completion of standing, surplus solution is filtered with 220 μm of miillpore filter, with 6 mL 20%
HCl wash twice；Suction filtration obtained solid is dispersed in the ultrapure water of 60 mL to ultrasound after stirring 2 h again, it is equal to obtain dispersion
Even solution adds it to the HCl of 40 mL 30%, stands 14 h；
(C) filtered with identical filter membrane and products therefrom is dispersed in again in 40 mL anhydrous methanols stirs 2 h, add 60 mL without
Water ether stands 1 h, then washs, is finally dispersed in obtained solid appropriate ultrapure with membrane filtration and with 10 mL ether
Ultrasound finally obtains stannic oxide/graphene nano band suspension to uniform in water, be freeze-dried can be in dark brown oxidation
Graphene nanobelt powder (GONRs).
The preparation of graphene oxide: after evenly mixing by graphite and the concentrated sulfuric acid/concentrated phosphoric acid system (v/v=9:1), slowly add
Enter potassium permanganate, after uniform stirring 0.5h, in 50 DEG C of stirred in water bath 12h, is slowly added to deionized water, and temperature is kept to be lower than
100 DEG C, the hydrogen peroxide of 5wt% is added dropwise, when mixed liquor becomes golden yellow, salt acid elution is added, reaction after five minutes, is spent
Ion water washing uses BaCl to neutrality2Detect the presence of SO4 2-Residual, then graphite oxide powder is made in freeze-drying for 24 hours；It will
Graphite oxide powder obtained is add to deionized water, then ultrasonic 1h is centrifuged 10min under the revolving speed of 2000r/min, goes
Except lower sediment thing, upper liquid is taken, after upper liquid is freezed 12h at 0 DEG C, is placed in freeze drier and is freeze-dried
36h obtains the graphene oxide.
Embodiment 1
A kind of preparation method of N and S codope graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) graphene oxide made from stannic oxide/graphene nano band made from 50mg step (1) and 50mg step (2) is taken to mix
Afterwards, 50mL deionized water is added, the mixed liquor that concentration is 2mg/mL is obtained after ultrasound is uniform；
(4) pyrroles of 0.5mg and the thiophene of 0.5mg are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction,
Reaction temperature is 165 DEG C, and reaction time 5h obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2M3In solution, secondary hydro-thermal reaction, reaction temperature 120 are carried out
DEG C, reaction time 3h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) by products therefrom thermal cracking 2h at 1050 DEG C in argon atmosphere after step (5) freeze-drying, the N and S is made
Codope graphene-graphene nanobelt aeroge.
Embodiment 2
A kind of preparation method of N and S codope graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) graphene oxide made from stannic oxide/graphene nano band made from 50mg step (1) and 50mg step (2) is taken to mix
Afterwards, 50mL deionized water is added, the mixed liquor that concentration is 2mg/mL is obtained after ultrasound is uniform；
(4) pyrroles of 0.5mg and the thiophene of 0.5mg are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction,
Reaction temperature is 180 DEG C, and reaction time 3h obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2M3In solution, secondary hydro-thermal reaction, reaction temperature 130 are carried out
DEG C, reaction time 2h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) by products therefrom thermal cracking 2h at 1100 DEG C in argon atmosphere after step (5) freeze-drying, the N and S is made
Codope graphene-graphene nanobelt aeroge.
Embodiment 3
A kind of preparation method of N and S codope graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) graphene oxide made from stannic oxide/graphene nano band made from 50mg step (1) and 50mg step (2) is taken to mix
Afterwards, 50mL deionized water is added, the mixed liquor that concentration is 2mg/mL is obtained after ultrasound is uniform；
(4) pyrroles of 0.5mg and the thiophene of 0.5mg are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction,
Reaction temperature is 170 DEG C, and reaction time 4h obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2M3In solution, secondary hydro-thermal reaction, reaction temperature 125 are carried out
DEG C, reaction time 2.5h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) by products therefrom thermal cracking 2h at 1080 DEG C in argon atmosphere after step (5) freeze-drying, the N and S is made
Codope graphene-graphene nanobelt aeroge.
Comparative example 1
A kind of preparation method of N doped graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) graphene oxide made from stannic oxide/graphene nano band made from 50mg step (1) and 50mg step (2) is taken to mix
Afterwards, 50mL deionized water is added, the mixed liquor that concentration is 2mg/mL is obtained after ultrasound is uniform；
(4) pyrroles of 0.5mg and the thiophene of 0.5mg are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction,
Reaction temperature is 170 DEG C, and reaction time 4h obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2M3In solution, secondary hydro-thermal reaction, reaction temperature 125 are carried out
DEG C, reaction time 2.5h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) by products therefrom thermal cracking 2h at 1080 DEG C in argon atmosphere after step (5) freeze-drying, the N is made and mixes
Miscellaneous graphene-graphene nanobelt aeroge.
Comparative example 2
A kind of preparation method of S doped graphene-graphene nanobelt aeroge, specifically includes the following steps:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) graphene oxide made from stannic oxide/graphene nano band made from 50mg step (1) and 50mg step (2) is taken to mix
Afterwards, 50mL deionized water is added, the mixed liquor that concentration is 2mg/mL is obtained after ultrasound is uniform；
(4) pyrroles of 0.5mg and the thiophene of 0.5mg are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction,
Reaction temperature is 170 DEG C, and reaction time 4h obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2M3In solution, secondary hydro-thermal reaction, reaction temperature 125 are carried out
DEG C, reaction time 2.5h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) by products therefrom thermal cracking 2h at 1080 DEG C in argon atmosphere after step (5) freeze-drying, the S is made and mixes
Miscellaneous graphene-graphene nanobelt aeroge.
N and S codope graphene-graphene nanobelt aeroge obtained above, N doped graphene-graphene are received
Rice band aeroge and S doped graphene-graphene nanobelt aeroge are used in electrode material, specific steps are as follows: N and S is bis-
Doped graphene/carbon nanotube aerogel (or N doped graphene-graphene nanobelt aeroge, S doped graphene-graphene
Nanobelt aeroge), acetylene black, ptfe emulsion be added in same weighing bottle according to the ratio that mass ratio is 90:5:5,
It is uniformly mixed and sample is blown to paste with hair dryer, using nickel foam as collector, pastes is coated to nickel foam
On, it is dried in vacuo at 120 DEG C for 24 hours, it is final that required electrode is made.
Electrode obtained is subjected to density, specific surface area and electrochemical property test, the results are shown in Table 1.
The properties of 1 silica aerogel electrode of table
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with repair
Decorations, are all covered by the present invention.
Claims (4)
1. a kind of preparation method of N and S codope graphene-graphene nanobelt aeroge, it is characterised in that: specifically include with
Lower step:
(1) preparation of stannic oxide/graphene nano band；
(2) preparation of graphene oxide；
(3) after mixing graphene oxide made from stannic oxide/graphene nano band made from step (1) and step (2), addition is gone
Ionized water obtains the mixed liquor that concentration is 2 mg/mL after ultrasound is uniform；
(4) pyrroles and thiophene are added into the mixed liquor that step (3) obtains, carries out a hydro-thermal reaction, reaction temperature is 165 ~
180 DEG C, the reaction time is 3 ~ 5 h, obtains hydrogel；
(5) hydrogel that step (4) obtains is put into the KNO of 2 M3In solution, secondary hydro-thermal reaction, reaction temperature 120 are carried out
~ 130 DEG C, the reaction time is 2 ~ 3 h, after being cooled to room temperature, using filter, washing and freeze-drying；
(6) it by products therefrom 2 h of thermal cracking at 1050 ~ 1100 DEG C in argon atmosphere after step (5) freeze-drying, is made
N the and S codope graphene-graphene nanobelt aeroge.
2. the preparation method of N and S codope graphene-graphene nanobelt aeroge according to claim 1, feature
Be: the mass ratio of stannic oxide/graphene nano band described in step (3) and graphene oxide is 1:1.
3. the preparation method of N and S codope graphene-graphene nanobelt aeroge according to claim 1, feature
Be: the mass ratio of pyrroles described in step (4) and thiophene is 1:1, and wherein the additional amount of pyrroles is graphene oxide
1wt%。
4. N and S codope graphene-graphene nanobelt aeroge made from a kind of preparation method as described in claim 1
Application in electrode material, it is characterised in that: by N and S codope graphene-graphene nanobelt aeroge, acetylene black, gather
Tetrafluoroethene lotion in the same weighing bottle of ratio addition of 90:5:5, is uniformly mixed according to mass ratio and will with hair dryer
Sample is blown to paste, and using nickel foam as collector, pastes is coated in nickel foam, is dried in vacuo at 120 DEG C for 24 hours,
It is final that required electrode is made.
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| CN201810841851.7A CN109003826B (en) | 2018-07-27 | 2018-07-27 | preparation method of N and S double-doped graphene-graphene nanoribbon aerogel |
| PCT/CN2018/108554 WO2020019507A1 (en) | 2018-07-27 | 2018-09-29 | Preparation method for n/s-double doped graphene – graphene nanoribbon aerogel |
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| CN110155992A (en) * | 2019-06-14 | 2019-08-23 | 福州大学 | A kind of preparation method of the sulfur and nitrogen co-doped graphene quantum dot electrolyte suitable for supercapacitor |
| CN111484644A (en) * | 2020-04-17 | 2020-08-04 | 东华理工大学 | Method for preparing, separating and enriching uranium from polyamidoxime/graphene nanoribbon composite aerogel |
| CN112795801A (en) * | 2020-12-28 | 2021-05-14 | 西南交通大学 | Preparation method of graphene-based reinforced carbon-copper composite material |
| CN115414874A (en) * | 2022-08-31 | 2022-12-02 | 安普瑞斯（无锡）有限公司 | Multiple polyatomic co-doped carbon aerogel and preparation method and application thereof |
| CN115472440A (en) * | 2022-08-18 | 2022-12-13 | 兰州大学 | Graphene-based N, S doped electrode material and preparation method thereof |
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| Publication number | Publication date |
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| WO2020019507A1 (en) | 2020-01-30 |
| CN109003826B (en) | 2019-12-17 |
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