CN104466133B - A kind of graphene carbon composite of N doping and preparation method thereof - Google Patents
A kind of graphene carbon composite of N doping and preparation method thereof Download PDFInfo
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- CN104466133B CN104466133B CN201410719551.3A CN201410719551A CN104466133B CN 104466133 B CN104466133 B CN 104466133B CN 201410719551 A CN201410719551 A CN 201410719551A CN 104466133 B CN104466133 B CN 104466133B
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
Graphene carbon composite that the invention discloses a kind of N doping and preparation method thereof.This composite includes nitrogen-doped graphene and the nitrogen-doped carbon material being coated on around nitrogen-doped graphene；This preparation method includes: be dissolved in graphene oxide dispersion by carbohydrate, and makes described carbohydrate uniformly be coated with graphene oxide, forms graphene oxide/carbohydrate compound；At described graphene oxide/carbohydrate compound surface parcel polymer, form graphene oxide/carbohydrate/polymer complex, and, described graphene oxide/carbohydrate/polymer complex is nitrogenized in the hot environment of more than 700 DEG C, forms the graphene carbon composite of described N doping.The composite specific surface area of the present invention is big, reunites few, favorable dispersibility, and electrical conductivity is good, and its preparation is simple, it is not necessary to lyophilization operates, and energy consumption is low, and yield is high, is suitable to large-scale industrial and produces.
Description
Technical field
The present invention relates to a kind of conductive carbon material, particularly to the graphene carbon composite of a kind of N doping, belong to material science.
Background technology
Graphene, due to the two-dimentional monolayer structure of its uniqueness and excellent physical property (high theoretical specific surface area, high conductivity, high-mechanical property etc.), is with a wide range of applications in lithium ion battery and electrode material for super capacitor.For obtaining the graphene-based material with more preferably electric property, industry have studied kinds of schemes, such as, a kind of mode therein is to utilize the method for physical mixed to prepare graphene composite material to improve its electric property, and the most feasible mode of another kind is chemical modification method, such as in grapheme material, introduce other element by doping grade, particularly N element and improve its electric property, owing to atom N has and the atomic radius of C atom approximation, and can be as electron donor, the nitrogen-doped graphene generated after adulterating with Graphene shows higher electric conductivity.
At present the method for N doping is carried out for Graphene and mainly have chemical gaseous phase deposition (CVD) method, plasma processing, arc discharge method, high energy electrothermal way, template etc..But because the most easily reuniting between sheet and the sheet of graphite alkenes material, particularly nitrogen-doped graphene, cause its electric property to reduce, so typically using cryodesiccated method to prepare the nitrogen-doped graphene of bigger serface, but Freeze Drying Technique yields poorly, energy consumption is high, is not suitable for industrialized production.
Summary of the invention
In view of the deficiencies in the prior art, present invention is primarily targeted at the graphene carbon composite that a kind of N doping is provided, the advantages such as it is big that it has specific surface area, and dispersion is high, electric property is excellent.
A kind of method that another object of the present invention is to provide graphene carbon composite preparing described N doping, the method is simple to operation, and energy consumption is low, and yield is high, is suitable to large-scale industrial and produces.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
A kind of graphene carbon composite of N doping, including nitrogen-doped graphene and the nitrogen-doped carbon material that is coated on around nitrogen-doped graphene, and the thickness of described nitrogen-doped carbon material is 2-10 nm, a diameter of 2-20 m of described composite, thickness is 5-20 nm, and electrical conductivity is 100-200 S/cm2, specific surface area is 200-300 m2/g。
Wherein, material with carbon element is unformed form.
Further, the nitrogen content in the graphene carbon composite of described N doping is 2-15mol%.
The preparation method of the graphene carbon composite of a kind of N doping includes:
Can be more than 700 DEG C, preferably at a temperature of 700-900 DEG C, the carbohydrate of carbonization is dissolved in graphene oxide dispersion, and makes described carbohydrate uniformly be coated with graphene oxide, forms graphene oxide/carbohydrate compound；
Described graphene oxide/carbohydrate compound surface parcel can at a temperature of 700-900 DEG C the polymer of carbonization, form graphene oxide/carbohydrate/polymer complex,
And, described graphene oxide/carbohydrate/polymer complex is nitrogenized in the hot environment of 700-900 DEG C, forms the graphene carbon composite of described N doping.
As more one of preferred embodiment, the preparation method of the graphene carbon composite of described N doping comprises the steps:
(1) it is sufficiently mixed in described carbohydrate being dissolved in the aqueous solution of graphene oxide, make described carbohydrate uniformly be coated with graphene oxide and form graphene oxide/carbohydrate compound, more described graphene oxide/carbohydrate compound is isolated from aqueous solution；
(2) described graphene oxide/carbohydrate compound is dispersed in water, and add the monomer of described polymer, after being sufficiently mixed, add acidic materials and catalyst, the monomer polymerization making described polymer forms polymer, and make described polymer uniform wrap up described graphene oxide/carbohydrate compound, form graphene oxide/carbohydrate/polymer complex, again described graphene oxide/carbohydrate/polymer complex is isolated from reactant mixture, and wash, be dried；
(3) described graphene oxide/carbohydrate/polymer complex is placed in nitrogen containing atmosphere, nitrogenizes under the temperature conditions more than 700 DEG C, form the graphene carbon composite of described N doping.
Further, abovementioned steps (1) including: is thoroughly mixed in described carbohydrate is dissolved in the aqueous solution of graphene oxide, add ammonia, stirring more than 2h is continued at 80-95 DEG C, it is subsequently adding CTAB and continues stirring, then leach precipitum, wash, be vacuum dried, it is thus achieved that described graphene oxide/carbohydrate compound.
Further, abovementioned steps (3) including: is placed in inert atmosphere by described graphene oxide/carbohydrate/polymer complex, and it is passed through ammonia, it is warming up to 700-900 DEG C with the heating rate of 10-30 DEG C/min, and nitrogenize under this temperature conditions, form the graphene carbon composite of described N doping.
Further, described carbohydrate is selected from but is not limited to glucose, fructose or sucrose.
Further, described polymer preferably is selected from polypyrrole.
Further, abovementioned steps (2) including: is dispersed in water by described graphene oxide/carbohydrate compound, and add the monomer of described polymer, after being sufficiently mixed, add acidic materials (such as hydrochloric acid, but it is not limited to this), the pH value of regulation mixture system, to 1-2, is beneficial to subsequent polymerisation reaction.
Further, described catalyst includes persulfate, such as Ammonium persulfate..
Such as, in a more typical case study on implementation, the preparation method of the graphene carbon composite of a kind of N doping includes: the glucose of 1-25g joins in the graphene oxide water solution of 1000ml (concentration is 0.2-5 mg mL-1), stir 30 minutes, rotating speed 100-300 rev/min.It is subsequently adding the ammonia spirit (25-28%) of 1-25ml, at 95 DEG C, continues stirring 2 hours.It is subsequently adding the CTAB(hexadecyltrimethylammonium of 20-500mg
Bromide, cetyl trimethylammonium bromide), filter after stirring ten minutes, washing.60 DEG C are dried 12 hours under vacuo, obtain graphene oxide/glucose mixture.Take ultrasonic 30 minutes of the graphene oxide/glucose mixture of 100mg, power 100W, it is dispersed in 100 ml water, add the pyrroles of 0.1 ml, stir 30 minutes, add the concentrated hydrochloric acid solution of 0.1 ml, more ultrasonic 5 minutes, it is subsequently adding the aqueous solution of the Ammonium persulfate. (1 mmol) of 5ml, reacts 2 hours at 0 DEG C.Then product is filtered, washing, vacuum drying.Product, under the atmosphere of argon, is passed through ammonia, and 700 DEG C of ammonifications 30 minutes, heating rate is 30 DEG C/min.
It is few that the present invention need not use lyophilization just can prepare reunion, the graphene/carbon material of the N doping that surface area is big, its principle is: graphene oxide good dispersion in aqueous, in aqueous with carbohydrate, surface of graphene oxide is coated with by such as glucose uniformly, further preferably settled down by CTAB etc., convenient filtration or centrifugation, the most again at graphene oxide/carbohydrate Surface coating one layer of polymeric, such as polypyrrole, during high-temperature ammonolysis graphene oxide/glucose/polypyrrole complex, glucose and polypyrrole etc. can produce gas, oxygen Graphene is stoped to be reunited, and under nitrogen effect, form the graphene/carbon composite material of N doping.
Compared with prior art, the invention have the advantages that the graphene carbon composite specific surface area of this N doping is big, reunite few, favorable dispersibility; electrical conductivity is high, and its preparation is simple, it is not necessary to lyophilization operates; energy consumption is low, and yield is high, is suitable to large-scale industrial and produces.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the carbon pipe/carbon fiber complex carbon material of the obtained hierarchy of embodiment 1；
Fig. 2 is the SEM figure of the carbon pipe/carbon fiber complex carbon material of the obtained hierarchy of embodiment 2；
Fig. 3 is the SEM figure of the carbon pipe/carbon fiber complex carbon material of the obtained hierarchy of embodiment 3；
Fig. 4 is that the XPS of the carbon pipe/carbon fiber complex carbon material of the obtained hierarchy of embodiment 1 tests collection of illustrative plates.
Detailed description of the invention
Below in conjunction with some embodiments and accompanying drawing, technical scheme is further described.
Embodiment 1 The glucose of 1g joins in the graphene oxide water solution of 1000ml that (concentration is 0.2 mg mL-1), stir 30 minutes, rotating speed 100-300 rev/min.It is subsequently adding the ammonia spirit (25-28%) of 1ml, at 95 DEG C, continues stirring 2 hours.It is subsequently adding the CTAB of 20mg, filters after stirring ten minutes, washing.60 DEG C are dried 12 hours under vacuo, obtain graphene oxide/glucose mixture.Take ultrasonic 30 minutes of the graphene oxide/glucose mixture of 100mg, power 100W, it is dispersed in 100 ml water, add the pyrroles of 0.1 ml, stir 30 minutes, add the concentrated hydrochloric acid solution of 0.1 ml, more ultrasonic 5 minutes, it is subsequently adding the aqueous solution of the Ammonium persulfate. (1 mmol) of 5ml, reacts 2 hours at 0 DEG C.Then product is filtered, washing, lyophilization.Product, under the atmosphere of argon, is passed through ammonia, and 700 DEG C of ammonifications 30 minutes, heating rate is 30 DEG C/min.Pattern as it is shown in figure 1, material with carbon element is coated on around nitrogen-doped graphene, thickness about 5 nm, electrical conductivity 200 S/cm2, surface area is 300 m2/g.Fig. 4 is the XPS test of composite, it can be seen that nitrogen mixes in complex.
Embodiment 2 The glucose of 25g joins in the graphene oxide water solution of 1000ml that (concentration is 5 mg mL-1), stir 30 minutes, rotating speed 100-300 rev/min.It is subsequently adding the ammonia spirit (25-28%) of 25ml, at 95 DEG C, continues stirring 2 hours.It is subsequently adding the CTAB of 500mg, filters after stirring ten minutes, washing.60 DEG C are dried 12 hours under vacuo, obtain graphene oxide/glucose mixture.Take ultrasonic 30 minutes of the graphene oxide/glucose mixture of 100mg, power 100W, it is dispersed in 100 ml water, add the pyrroles of 0.1 ml, stir 30 minutes, add the concentrated hydrochloric acid solution of 0.1 ml, more ultrasonic 5 minutes, it is subsequently adding the aqueous solution of the Ammonium persulfate. (1 mmol) of 5ml, reacts 2 hours at 0 DEG C.Then product is filtered, washing, lyophilization.Product, under the atmosphere of argon, is passed through ammonia, and 750 DEG C of ammonifications 30 minutes, heating rate is 30 DEG C/min.Pattern is as in figure 2 it is shown, material with carbon element is coated on around nitrogen-doped graphene, and thickness is 10 nm, electrical conductivity 160 S/cm2, surface area is 250 m2/g。
Embodiment 3 The glucose of 10g joins in the graphene oxide water solution of 1000ml that (concentration is 2 mg mL-1), stir 30 minutes, rotating speed 100-300 rev/min.It is subsequently adding the ammonia spirit (25-28%) of 10 ml, at 95 DEG C, continues stirring 2 hours.It is subsequently adding the CTAB of 200mg, filters after stirring ten minutes, washing.60 DEG C are dried 12 hours under vacuo, obtain graphene oxide/glucose mixture.Take ultrasonic 30 minutes of the graphene oxide/glucose mixture of 100mg, power 100W, it is dispersed in 100 ml water, add the pyrroles of 0.1 ml, stir 30 minutes, add the concentrated hydrochloric acid solution of 0.1 ml, more ultrasonic 5 minutes, it is subsequently adding the aqueous solution of the Ammonium persulfate. (1 mmol) of 5ml, reacts 2 hours at 0 DEG C.Then product is filtered, washing, lyophilization.Product, under the atmosphere of argon, is passed through ammonia, and 750 DEG C of ammonifications 30 minutes, heating rate is 30 DEG C/min.Pattern is as it is shown on figure 3, material with carbon element is coated on around nitrogen-doped graphene, and thickness is 20 nm, electrical conductivity 120 S/cm2, surface area is 200 m2/g。
It should be pointed out that, the detailed description of the invention of present invention described above, be not intended that limiting the scope of the present invention.Any according to other changes accordingly various done by the technology design of the present invention and deformation, should be included in the protection domain of the claims in the present invention.
Claims (10)
1. the preparation method of the graphene carbon composite of a N doping, it is characterised in that including:
To can be dissolved in the aqueous solution of graphene oxide by the carbohydrate of carbonization at a temperature of 700 DEG C-900 DEG C, and make described carbohydrate uniformly be coated with graphene oxide, form graphene oxide/carbohydrate compound；
Described graphene oxide/carbohydrate compound surface parcel can at a temperature of 700-900 DEG C the polymer of carbonization, form graphene oxide/carbohydrate/polymer complex,
And, described graphene oxide/carbohydrate/polymer complex is nitrogenized in the hot environment of 700-900 DEG C, form the graphene carbon composite of N doping, the graphene carbon composite of described N doping includes nitrogen-doped graphene and the nitrogen-doped carbon material being coated on around nitrogen-doped graphene, and the thickness of described nitrogen-doped carbon material is 2-10 nm, a diameter of 2-20 m of described composite, thickness is 5-20 nm, and electrical conductivity is 100-200 S/cm , specific surface area is 200-300 m2/g。
The preparation method of the graphene carbon composite of N doping the most according to claim 1, it is characterised in that comprise the steps:
(1) it is sufficiently mixed in described carbohydrate being dissolved in the aqueous solution of graphene oxide, make described carbohydrate uniformly be coated with graphene oxide and form graphene oxide/carbohydrate compound, more described graphene oxide/carbohydrate compound is isolated from aqueous solution；
(2) described graphene oxide/carbohydrate compound is dispersed in water, and add the monomer of described polymer, after being sufficiently mixed, add acidic materials and catalyst, the monomer polymerization making described polymer forms polymer, and make described polymer uniform wrap up described graphene oxide/carbohydrate compound, form graphene oxide/carbohydrate/polymer complex, again described graphene oxide/carbohydrate/polymer complex is isolated from reactant mixture, and wash, be dried；
(3) described graphene oxide/carbohydrate/polymer complex is placed in nitrogen containing atmosphere, nitrogenizes under the temperature conditions of 700 DEG C-900 DEG C, form the graphene carbon composite of described N doping.
The preparation method of the graphene carbon composite of N doping the most according to claim 2, it is characterized in that, step (1) including: is thoroughly mixed in described carbohydrate is dissolved in the aqueous solution of graphene oxide, add ammonia, stirring more than 2h is continued at 80-95 DEG C, it is subsequently adding CTAB and continues stirring, then leach precipitum, wash, be vacuum dried, it is thus achieved that described graphene oxide/carbohydrate compound.
The preparation method of the graphene carbon composite of N doping the most according to claim 2, it is characterized in that, step (3) including: is placed in inert atmosphere by described graphene oxide/carbohydrate/polymer complex, and it is passed through ammonia, it is warming up to 700-900 DEG C with the heating rate of 10-30 DEG C/min, and nitrogenize under this temperature conditions, form the graphene carbon composite of described N doping.
5. according to the preparation method of the graphene carbon composite of N doping according to any one of claim 1-3, it is characterised in that: described carbohydrate includes glucose, fructose or sucrose.
6. according to the preparation method of the graphene carbon composite of N doping according to any one of claim 1-3, it is characterised in that: described polymer includes polypyrrole.
The preparation method of the graphene carbon composite of N doping the most according to claim 2, it is characterized in that, step (2) including: is dispersed in water by described graphene oxide/carbohydrate compound, and add the monomer of described polymer, after being sufficiently mixed, add acidic materials, the pH value of regulation mixture system to 1-2.
8. according to claim 2-3, the preparation method of the graphene carbon composite of N doping according to any one of 7, it is characterised in that: described acidic materials include hydrochloric acid.
9. according to the preparation method of the graphene carbon composite of N doping according to any one of claim 2-3, it is characterised in that: described catalyst includes persulfate.
The preparation method of the graphene carbon composite of N doping the most according to claim 9, it is characterised in that: described persulfate includes Ammonium persulfate..
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| CN106328904B (en) * | 2016-10-26 | 2019-01-29 | 北京光科博冶科技有限责任公司 | Height ratio capacity nitrogen-doped graphene nickle cobalt lithium manganate composite material and preparation method |
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