CN104710445A - Boron and nitrogen codoped graphene, and preparation method and application thereof - Google Patents
Boron and nitrogen codoped graphene, and preparation method and application thereof Download PDFInfo
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Abstract
Boron and nitrogen codoped graphene has a lamellar folded structure, and the lamellar number is 1-10; boron and nitrogen are in the molecular crystal lattice structure of graphene; boron and nitrogen are in different graphene six-membered rings, and one of the graphene six-membered rings contains one boron atom or one nitrogen atom; or one boron atom and one nitrogen atom are in a same graphene six-membered ring. The graphene is prepared through a two-step heating and heat insulation method under inert conditions Compared with the prior art, the method has the advantages of simplicity, easy implementation, no need of a catalyst in the preparation process, easy control of the reaction process, and suitableness for large scale production. Additionally, boron and nitrogen codoped graphene prepared through adopting the method has an advantage that the structure of doping elements in graphite crystal lattice can be regulated. The boron and nitrogen codoped graphene in a separate state maintains the doping inherent characters of boron and nitrogen, and is a good electrocatalysis material; and the boron and nitrogen codoped graphene in a combined state can be used as a dielectric material.
Description
Technical field
The present invention relates to a kind of boron, nitrogen co-doped Graphene, the present invention also relates to the preparation method of boron, nitrogen co-doped Graphene simultaneously.
Background content
Owing to there is wide application prospect, the graphene film layer material with graphite-structure is just being subject to more and more studying concern.Compare graphite and hexagonal boron nitride material, Graphene three component system material has the adjustable advantage of composition and structure.The performance of this three component system material is decided by doping content and their structure of boron and nitrogen to a great extent.In grapheme material system, they can be divided into two classes: namely boron and nitrogen are in the boron of ortho position combined, nitrogen co-doped Graphene by the relative position in lattice according to boron and nitrogen, and non-ortho position is separated boron, the nitrogen co-doped Graphene of state.Due to the difference of structure, there is larger difference in this bi-material in performance.At present, the preparation of graphene film layer material mainly adopts chemical Vapor deposition process.The shortcoming of this method is that grapheme material boron atom and nitrogen-atoms in process of growth easily combine and form boron, nitrogen co-doped Graphene, is unsuitable for preparing boron, nitrogen co-doped grapheme material, and is difficult to realize mass.In order to control boron and nitrogen-atoms structure in grapheme material and form non-ortho position Graphene, some research groups have developed " two step doping methods " prepares grapheme material.The feature of " two step doping methods " is, first adulterate a kind of element in parent graphite lattice, and then mix another element.Because the element first mixed is surrounded by carbon atom, the element be difficult to follow-up doping combines, and forms grapheme material.In order to find the more easy method preparing grapheme material, we have developed a kind of " soft template " method to prepare graphene nano sheet layer material.The feature of this preparation method is to adopt polymerisable nitrogenous compound (as urea, nitrile amine, trimeric cyanamide etc.), with can the compound of carbonization (as carbohydrate, high polyalcohols etc.) and boron precursor (as boric acid, boron oxide compound) Homogeneous phase mixing after, make nitrogenous compound aggregate into lamellar compound g-C first at a lower temperature
3n
4" soft template ", simultaneously the presoma of carbon is in its interlayer carbonization.At higher temperatures, g-C
3n
4soft template is decomposed and forms the graphite-structure of lamella.G-C
3n
4degradation production can be used for the doping of nitrogen, boric acid is then for doped with boron.By adjustment pyroprocessing condition, boron can be prepared respectively, nitrogen is co-located in combined and the Graphene of point amorph.
Summary of the invention
For achieving the above object, the present invention adopts following concrete mode to realize.
A kind of boron, nitrogen co-doped Graphene, described Graphene is lamella fold-like structures, and the number of plies of lamella is between 1-10 layer; Boron doping amount is 1%-16.6%, and N doping amount is 1%-16.6%.
Described boron and nitrogen are in the molecular lattice structure of Graphene; Boron and nitrogen are in different Graphene six-rings, there is a boron or a nitrogen in a Graphene six-ring; Or a boron and a nitrogen are in same Graphene six-ring.
The preparation method of described boron, nitrogen co-doped Graphene, comprises following preparation process,
A) by the presoma of carbon, nitrogen and boron mixing and stirring in solvent, wherein, in presoma, the mol ratio of carbon and nitrogen is 1:5-1:120; In presoma, the mol ratio of carbon and boron is 1:0.01:-1:1;
B), after a) gained mixture is dried in 60 DEG C by step, under protection of inert gas, under 450-650 DEG C of condition, 0.5-24h is incubated;
C) by step b) products therefrom, under protection of inert gas, be heated to 700-1100 DEG C further and be incubated 0.5-24h, after being cooled to room temperature, obtaining boron, nitrogen co-doped Graphene.
Step b) described in holding temperature more excellent be 550-600 DEG C; Soaking time is more excellent is 2-4h; Step c) described in holding temperature more excellent be 800-1000 DEG C; Soaking time is more excellent is 2-4h.
When the mol ratio of the presoma of carbon described in step a) and nitrogen is 1:5-1:120, the presoma of carbon and boron mole be 1:0.01-1:0.25; Step c) described in Heating temperature under protection of inert gas be 950-1100 DEG C, in now obtained Graphene, if when a boron and a nitrogen are in same Graphene six-ring, boron and nitrogen are in contraposition point amorph in the molecular structure.
When the mol ratio of the presoma of carbon described in step a) and nitrogen is 1:5-1:120, the mol ratio of the presoma of carbon and boron is 1:0.01-1:1; Step c) described in Heating temperature under protection of inert gas be 700-850 DEG C, in now obtained Graphene, if when a boron and a nitrogen are in same Graphene six-ring, boron and nitrogen are in ortho position combined in the molecular structure.
Step a) described in the presoma of carbon be one or more in sucrose, glucose, polyoxyethylene glycol, Mierocrystalline cellulose; The presoma of described nitrogen is one or more in urea, nitrile amine, trimeric cyanamide; The presoma of described boron is boric acid or boron oxide or the mixture of the two.
Step a) described in solvent be ethanol or water or both mixtures.
Step b) and step c) described in rare gas element be one or more in nitrogen, argon gas, helium.
The application of the codoped Graphene that prepared by described method state boron, nitrogen is in contraposition, it can be used for the oxygen reduction electro-catalyst in alkaline environment.
The application of the codoped Graphene that prepared by described method state boron, nitrogen is in ortho position, it can be used for dielectric materials.
Compared with prior art, the Graphene of boron of the present invention and N doping has the following advantages: the structure of doped element in graphite lattice can regulate and control.The boron of separate stage obtained and the Graphene of N doping, can keep the doping person's character of boron and nitrogen, be a kind of good electrocatalysis material.The boron obtained and the Graphene of nitrogen bonding state, can be used as dielectric materials.Prepared Graphene has pleated structure, and it can be stoped to reunite.The method is simple, and preparation process is without the need to catalyzer, and to equipment without particular requirement, reaction process is easy to control, and is suitable for scale operation.
Accompanying drawing explanation
Fig. 1 graphene film layer material STEM schemes and elemental line scan;
The AFM figure of Fig. 2 graphene film layer material;
The Raman collection of illustrative plates of the graphene film layer material prepared under Fig. 3 different condition;
The infrared spectra of graphene film layer material is prepared under Fig. 4 different condition;
The oxygen reduction catalytic activity of graphene film layer material is prepared under Fig. 5 different condition.
Embodiment
Embodiment 1:
1) by sucrose, urea and boric acid are according to ratio Homogeneous phase mixing in ethanol of mol ratio 1:120:0.25;
2), after being dried in 60 DEG C by step a) gained mixture, under 550 DEG C of nitrogen, condition is incubated 4 hours;
3) by step b) products therefrom, be warming up under nitrogen protection condition 1000 DEG C of insulations 2 hours, obtain boron, nitrogen co-doped Graphene after being cooled to room temperature, be labeled as acquisition Graphene-2.5-1000.
Characterize the pattern of products therefrom and structure, result as shown in Figure 1-2.As can be seen from the figure, the Graphene obtained has laminated structure, and the thickness of lamella is below 4 nanometers, and the corresponding number of plies is 1-10 layer, and lamella has obvious coiled structure.Doped element is distributed in lamella inside uniformly.
Embodiment 2:
The present embodiment preparation method with embodiment 1, the sucrose wherein in step (1), urea and boric acid, according to mol ratio 1:120:1, obtain Graphene-10-1000 under the condition that other condition is constant;
Embodiment 3:
The present embodiment preparation method with embodiment 1, the sucrose wherein in step (1), urea and boric acid, according to mol ratio 1:120:0.1, obtain Graphene-1-1000 under the condition that other condition is constant;
Embodiment 4:
The present embodiment preparation method with embodiment 1, the sucrose wherein in step (1), the holding temperature of the 3rd step, according to mol ratio 1:120:0.25, is adjusted to 800 DEG C by urea and boric acid, under the condition that other condition is constant, obtain Graphene-2.5-800;
Embodiment 5:
The present embodiment preparation method with embodiment 1, the sucrose wherein in step (1), the holding temperature of the 3rd step, according to mol ratio 1:120:0.25, is adjusted to 900 DEG C by urea and boric acid, under the condition that other condition is constant, obtain Graphene-2.5-900;
As shown in Figure 3, all samples all shows obvious graphite features peak G peak (1580cm to the Raman spectrum of the sample prepared by embodiment 1-5
-1), and D peak is all obvious, the graphite platelet structure inside that surface obtains has a lot of defect.
The x-ray photoelectron power spectrum of the sample prepared by embodiment 1-5 is as shown in Figure 4, and as can be seen from the figure, all contain B in all samples, C and N element, result conforms to the EDX in scanning electron microscope.
The electrochemical catalysis activity of the sample prepared by embodiment 1-5 as shown in Figure 5.Hydrogen reduction test adopts diameter to be 0.15mm glass carbon rotating disk electrode, and the charge capacity of catalyzer is 80 micrograms.Test condition is room temperature condition, and electrolytic solution is 0.1M KOH, and reference electrode used is Ag/AgCl electrode.Can obviously find out from figure, there is obvious gap in the catalytic activity of the sample obtained, wherein the catalytic activity of Graphene-5-1000 and Graphene-2.5-800 is poor, and unadulterated graphite active is more or less the same.And Graphene-2.5-1000 and Graphene-1-1000 demonstrates the catalytic activity energy close with platinum.
Claims (11)
1. boron, a nitrogen co-doped Graphene, is characterized in that: described Graphene is lamella fold-like structures, and the number of plies of lamella is between 1-10 layer;
Boron doping amount is 1%-16.6%, and N doping amount is 1%-16.6%.
2. boron, nitrogen co-doped Graphene as claimed in claim 1, is characterized in that: boron and nitrogen are in the molecular lattice structure of Graphene;
Boron and nitrogen are in different Graphene six-rings, there is a boron or a nitrogen in a Graphene six-ring; Or a boron and a nitrogen are in same Graphene six-ring.
3. a preparation method for boron, nitrogen co-doped Graphene described in claim 1 or 2, is characterized in that: comprise following preparation process,
A) by the presoma of carbon, nitrogen and boron mixing and stirring in solvent, wherein, in presoma carbon and nitrogen mol ratio be 1:5-1:120; In presoma carbon and boron mol ratio be 1:0.01:-1:1;
B), after a) gained mixture is dried in 60 DEG C by step, under protection of inert gas, under 450-650 DEG C of condition, 0.5-24h is incubated;
C) by step b) products therefrom, under protection of inert gas, be heated to 700-1100 DEG C further and be incubated 0.5-24h, after being cooled to room temperature, obtaining boron, nitrogen co-doped Graphene.
4. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3, is characterized in that: step b) described in holding temperature more excellent be 550-600 DEG C; Soaking time is more excellent is 2-4h; Step c) described in holding temperature more excellent be 800-1000 DEG C; Soaking time is more excellent is 2-4h.
5. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3, is characterized in that: when the mol ratio of the presoma of carbon described in step a) and nitrogen is 1:5-1:120, the presoma of carbon and boron mole be 1:0.01-1:0.25;
Step c) described in Heating temperature under protection of inert gas be 950-1100 DEG C, in now obtained Graphene, if when a boron and a nitrogen are in same Graphene six-ring, boron and nitrogen are in contraposition point amorph in the molecular structure.
6. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3, is characterized in that: when the mol ratio of the presoma of carbon described in step a) and nitrogen is 1:5-1:120, the mol ratio of the presoma of carbon and boron is 1:0.01-1:1;
Step c) described in Heating temperature under protection of inert gas be 700-850 DEG C, in now obtained Graphene, if when a boron and a nitrogen are in same Graphene six-ring, boron and nitrogen are in ortho position combined in the molecular structure.
7. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3, is characterized in that: step a) described in the presoma of carbon be one or more in sucrose, glucose, polyoxyethylene glycol, Mierocrystalline cellulose; The presoma of described nitrogen is one or more in urea, nitrile amine, trimeric cyanamide; The presoma of described boron is boric acid or boron oxide or the mixture of the two.
8. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3: it is characterized in that: step a) described in solvent be ethanol or water or both mixtures.
9. the preparation method of boron, nitrogen co-doped Graphene as claimed in claim 3: it is characterized in that: step b) and step c) described in rare gas element be one or more in nitrogen, argon gas, helium.
10. an application for codoped Graphene described in claim 1 or 2, is characterized in that: the codoped Graphene that prepared by method described in claim 5 state boron, nitrogen is in contraposition can be used for the oxygen reduction electro-catalyst in alkaline environment.
The application of codoped Graphene described in 11. 1 kinds of claims 1 or 2, is characterized in that: the codoped Graphene that prepared by method described in claim 6 state boron, nitrogen is in ortho position can be used for dielectric materials.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105562050A (en) * | 2015-12-15 | 2016-05-11 | 华南理工大学 | Porous graphene-like structure doped carbon material as well as preparation method and application of porous graphene-like structure doped carbon material |
| CN105731437A (en) * | 2016-01-26 | 2016-07-06 | 苏州大学 | Exotic-atom-doped graphene, and preparation method and application thereof |
| CN106898774A (en) * | 2015-12-18 | 2017-06-27 | 中国科学院大连化学物理研究所 | One kind peels off carbon block and its preparation and application |
| CN108380231A (en) * | 2018-02-11 | 2018-08-10 | 青岛大学 | A method of preparing boron-nitrogen-carbon ternary material from carbonitride |
| CN108440236A (en) * | 2018-05-09 | 2018-08-24 | 福州大学 | A method of utilizing conductor photocatalysis hydrogenating reduction organohalogen compounds |
| CN108987559A (en) * | 2018-06-28 | 2018-12-11 | 江苏师范大学 | A kind of thermal management system for integrated circuit based on grapheme material |
| CN109110748A (en) * | 2018-11-07 | 2019-01-01 | 河南师范大学 | A kind of preparation method of nitrogen, the three-dimensional porous graphene of boron codope |
| CN109482214A (en) * | 2018-10-23 | 2019-03-19 | 深圳市本征方程石墨烯技术股份有限公司 | The catalyst and preparation method of a kind of graphene-supported ruthenium metal and application |
| CN109775692A (en) * | 2017-11-15 | 2019-05-21 | 南京理工大学 | The preparation method of heteroatom doped graphene |
| CN110010911A (en) * | 2019-03-14 | 2019-07-12 | 上海交通大学 | A kind of codope porous graphene cathode non-platinum catalyst and preparation method thereof |
| CN111170306A (en) * | 2020-01-10 | 2020-05-19 | 南昌大学 | Boron/nitrogen double-doped porous carbon nanosheet and lithium-sulfur battery positive electrode material thereof |
| CN111167503A (en) * | 2020-03-05 | 2020-05-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterojunction catalyst without metal component, product and application thereof |
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