CN105621393A - Functionalized graphene material, and preparation method and application thereof - Google Patents
Functionalized graphene material, and preparation method and application thereof Download PDFInfo
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- CN105621393A CN105621393A CN201410708174.3A CN201410708174A CN105621393A CN 105621393 A CN105621393 A CN 105621393A CN 201410708174 A CN201410708174 A CN 201410708174A CN 105621393 A CN105621393 A CN 105621393A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a multi-doped graphitized carbon material and a preparation method thereof. The graphitized carbon material has a lamellar structure, and is monolayer or multilayer graphene. Nitrogen is embedded to graphitized crystal lattices of the carbon material, and boron atoms are possibly embedded; and the edges of the carbon crystal lattices are modified with phosphorus and/or sulfur element function groups. The carbon material has advantages of strong hydrophilicity and good electricity conduction property, and has potential application values in electrocatalysis materials, super capacitor materials, lithium ion batteries and other electrode materials.
Description
Technical field
The present invention relates to a kind of graphitized carbon material, be modified with the graphitized carbon material of other atoms and group more particularly to carbon intracell and edge respectively;
The invention still further relates to the preparation method of above-mentioned graphitized carbon material and application.
Background technology
Graphene is as a kind of novel nano material, since it comes out, just becomes academia and the focus of industrial circle concern. Graphene has good intrinsic performance, for instance its theoretical specific surface area is up to 2630m2/ g, thermal conductivity reaches 5000W/mK, and theoretical charge migration rate is up to 200000cm2V-1s-1, Young's modulus reaches 1TPa. These performances make it have much potential using value at ambits such as electronics, biology, physics, materials.
Graphene also result in the extensive concern of academia and industrial circle as electrode material. Carbon as electrochemical electrode material, it is necessary to meet following primary condition: first, material with carbon element to have good intermiscibility with electrolyte, and material with carbon element itself is more stable, and not by electrolytic corrosion, meanwhile, also catalytic electrolysis liquid is not decomposed; Secondly, specific material to be had good chemism by it, and such as, as the material with carbon element of oxygen reduction electrode, oxygen molecule to be had good activation by it; Finally, material with carbon element to have good electric conductivity. Sum it up, material with carbon element should keep significantly high chemical inertness as electrode material, ensure its selective chemism again. For material with carbon element, the electronics of its chemically inert its delocalization that has its source in is more stable, it is difficult to the orbit coupling Cheng Jian of other material. By certain method active electronic, it is possible to be effectively improved the activity of these electronics, thus improving its intrinsic properties. By doping or finishing, Graphene being carried out functionalization is to the important channel that Graphene is modified. By adulterating, the performance of Graphene body being regulated and controled, research shows a lot of doped chemical, such as boron, nitrogen phosphate and sulfur etc., may be incorporated in Graphene lattice, changes its native electronic structure, form new electronic state, thus giving its new physical and chemical performance. And material with carbon element as electrode material stability problem main contributor in the carbon of marginal texture, the carbon of these positions is unsaturated due to coordination, is in metastable state, it is easy to is subject to ion attack and corrodes. Meanwhile, it also has good chemism, it is easy to the decomposition of catalytic electrolysis liquid. Therefore, reasonably construct the material with carbon element of high activity, high chemical compatibility, development high-performance carbon-based electrode material is had great importance.
The present invention, in order to obtain a kind of high-performance carbon-based electrode material, is prepared for the grapheme material of a kind of new construction. Its Graphene intracell doped with nitrogen or (with) boron. Then carry out functionalized process at the edge of Graphene, be modified with phosphate radical, polyphosphoric acid root or sulfonate ion. The hetero atom of these graphene-doped intracells; activate its electronics greatly; make it produce significantly high chemism, and the carbon atom being positioned at the Protect edge information that the phosphate radical at edge, polyphosphoric acid root or sulfonate ion can be significantly high is not corroded, it is ensured that the stability of material with carbon element. This material has good parents' performance (hydrophilic and oleophylic), chemical stability and electric conductivity, has potential using value as electrode materials such as eelctro-catalyst, super capacitor material, lithium ion battery electrode materials.
Summary of the invention
Graphitized carbon material of the present invention, its carbon intracell is embedded with nitrogen-atoms, it is possible to be embedded with boron atom; And carbon lattice fringe is modified with phosphorus and/or element sulphur functional group, its structure is as shown in drawings shown in 1-4: correspond respectively to nitrogen-doped graphene, and edge is modified with the Graphene (Fig. 1) of phosphate radical or polyphosphate ion; Nitrogen-doped graphene, edge is modified with the Graphene (Fig. 2) of sulfonate ion; Nitrogen and boron doped graphene, edge is modified with the Graphene (Fig. 3) of phosphate radical or polyphosphate ion; Nitrogen and boron doped graphene, edge simultaneously again phosphate radical or polyphosphate ion and sulfonic acid with the Graphene (Fig. 4) modified.
In described material with carbon element, the doped chemical of intracell can well active electronic; it is made to produce higher chemism; and the carbon atom being positioned at the Protect edge information that the phosphate radical at edge, polyphosphoric acid root or sulfonate ion can be significantly high is not corroded, it is ensured that the stability of material with carbon element. Simultaneously because the existence of these functional groups, this material can be made to have parents' performance (hydrophilic and oleophylic) chemical stability and electric conductivity, as electrode materials such as eelctro-catalyst, super capacitor material, lithium ion battery electrode materials, there is potential using value.
The present invention adopts scheme in detail below to realize:
A kind of intracell is doped with nitrogen element, and edge is modified with phosphate radical and the Graphene of sulfonate radical polyphosphate ion or sulfonate ion: comprise the following steps,
A tripolycyanamide is mixed by () with solubility carbon source, be simultaneously introduced acid source and stir to complete dissolve after rotary evaporation dry to obtain precipitate;
Described acid source is one or more and/or the phosphoric acid in sulphuric acid or sulphuric acid anhydride or one or more in phosphoric acid anhydride;
B step (a) gained precipitate high-temperature process in inert atmosphere is obtained carbon intracell and is embedded with nitrogen-atoms by (), carbon lattice fringe is modified with phosphorus and/or the graphitized carbon material of element sulphur functional group.
In described step (a), solubility carbon source is the one or more kinds of mixture in glucose, sucrose, fructose, maltose, lactose, crystal sugar, chitosan, polyvinyl alcohol, Polyethylene Glycol, soluble starch.
In described step (b), inert atmosphere is one or more in nitrogen, argon or helium.
In described step (b), the condition of high-temperature process is heat to 350-650 DEG C with 1-20 DEG C/min programming rate, is incubated 1-24 hour, then heats to 750-1100 DEG C with 1-20 DEG C/min programming rate, be incubated 1-24 hour.
In described step (b), phosphorus and/or element sulphur functional group are one or more in phosphate groups, sulfonate group, polyphosphoric acid foundation group.
In described step (a), the mol ratio of solubility carbon source and tripolycyanamide is 1:10-1:100, and the mol ratio of described acid source and tripolycyanamide is at 1:0.1-1:10.
Described sulphuric acid anhydride is SO3, phosphoric acid anhydride is P2O5Or the one or more than one in polyphosphoric acids.
A kind of intracell is doped with boron and nitrogen element, and edge is modified with phosphate radical and the Graphene of sulfonate radical polyphosphate ion or sulfonate ion: comprise the following steps,
A tripolycyanamide is mixed by () with solubility carbon source, be simultaneously introduced acid source and stir to complete dissolve after rotary evaporation dry to obtain precipitate;
Described acid source is one or more in boric acid or boric acid anhydride, and one or more and/or phosphoric acid in sulphuric acid or sulphuric acid anhydride or one or more in phosphoric acid anhydride;
B step (a) gained precipitate high-temperature process in inert atmosphere is obtained carbon intracell and is embedded with nitrogen and boron atom by (), carbon lattice fringe is modified with phosphorus and/or the graphitized carbon material of element sulphur functional group.
In described step (a), solubility carbon source is the one or more kinds of mixture in glucose, sucrose, fructose, maltose, lactose, crystal sugar, chitosan, polyvinyl alcohol, Polyethylene Glycol, soluble starch.
In described step (b), inert atmosphere is one or more in nitrogen, argon or helium.
In described step (b), the condition of high-temperature process is heat to 350-650 DEG C with 1-20 DEG C/min programming rate, is incubated 1-24 hour, then heats to 750-1100 DEG C with 1-20 DEG C/min programming rate, be incubated 1-24 hour.
In described step (b), phosphorus and/or element sulphur functional group are one or more in phosphate groups, sulfonate group, polyphosphoric acid foundation group.
In described step (a), the mol ratio of solubility carbon source and tripolycyanamide is 1:10-1:100, and the mol ratio of described acid source and tripolycyanamide is at 1:0.1-1:10.
Described sulphuric acid anhydride is SO3, phosphoric acid anhydride is P2O5Or the one or more than one in polyphosphoric acids.
Accompanying drawing explanation
Fig. 1 is nitrogen-doped graphene, and edge is modified with the schematic diagram of the Graphene of phosphate radical or polyphosphate ion;
Fig. 2 is nitrogen-doped graphene, and edge is modified with the schematic diagram of the Graphene of sulfonate ion;
Fig. 3 is nitrogen and boron doped graphene, and edge is modified with the schematic diagram of the Graphene of phosphate radical or polyphosphate ion;
Fig. 4 is nitrogen and boron doped graphene, edge simultaneously again phosphate radical or polyphosphate ion and sulfonic acid with the schematic diagram of the Graphene modified;
Fig. 5 is structure and the pattern of the Graphene of the N doping phosphate radical according to example 1 preparation or the modification of polyphosphoric acid root edge.
Fig. 6 is the hydrogen reduction catalytic performance of the Graphene preparing N doping phosphate radical or the modification of polyphosphoric acid root edge according to example 1.
Fig. 7 is the electrochemical capacitance performance of the Graphene preparing N doping phosphate radical or the modification of polyphosphoric acid root edge according to example 1.
Detailed description of the invention
Embodiment 1:
By the material made prepared by the present embodiment be intracell doped with nitrogen element, then there is the grapheme material that phosphate radical is modified at carbon edge. The doping content of nitrogen element is 4.3at%, and the concentration of P elements is 5.7at%. The structural representation of this material is as shown in Figure 1. Its preparation method is as follows:
A () adds mol ratio in 95 DEG C of deionized waters is the tripolycyanamide of 40:1, glucose, stirs and obtains mixed solution after being completely dissolved;
B () adds phosphoric acid in the described mixed solution of step (a), the mol ratio of phosphate radical and tripolycyanamide is 1:5, stirs to mix homogeneously rotary evaporation and dries and to obtain melamine phosphate precipitation;
C (), in tube furnace, under argon shield, is warming up to 560 DEG C with 10 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 20 DEG C/min again, is incubated 10 hours.
The pattern of the material with carbon element prepared by the present embodiment, structure and chemical composition are as shown in Figure 5. As it can be seen, prepared material with carbon element is macroscopically homogeneous graininess (Fig. 5 a), and under the SEM Electronic Speculum of high power, it can be seen that these granular granules are the lamellar structure (Fig. 5 b) peeled off. By transmission electron microscope it can be seen that these lamellas have a lot of fold, and above lamella, there is a lot of cavity (Fig. 5 c). High power transmission electron microscope photo shows, the interlamellar spacing of these lamellas is 0.34nm, for { the interlamellar spacing (Fig. 5 d) in 0001} face of typical carbon. By Raman spectrum it can also be seen that these materials have typical carbon structure (G peak), but there is a lot of defect (D peak is stronger) (Fig. 5 e) above. The material obtained has performance (Fig. 6) and the electrochemical capacitance performance (Fig. 7) of good catalytic oxidation-reduction
Embodiment 2:
By the material made prepared by the present embodiment be intracell doped with nitrogen element, then there is the grapheme material that sulfonate radical is modified at carbon edge. The doping content of nitrogen element is 8at%, and the concentration of element sulphur is 3.8at%. The structural representation of this material is as shown in Figure 1. Its preparation method is as follows:
A () adds mol ratio in 95 DEG C of deionized waters is the tripolycyanamide of 80:1, fructose, stirs and obtains mixed solution after being completely dissolved;
B () adds sulphuric acid in the described mixed solution of step (a), the mol ratio of sulfate radical and tripolycyanamide is 1:10, stirs to mix homogeneously rotary evaporation and dries and to obtain melamine phosphate precipitation;
C (), in tube furnace, under nitrogen protection, is warming up to 380 DEG C with 5 DEG C/min, be incubated 2.5 hours, be then warming up to 950 DEG C with 2 DEG C/min again, is incubated 3 hours.
Embodiment 3:
By the material made prepared by the present embodiment be intracell doped with nitrogen and boron element, then there is the grapheme material that phosphate radical is modified at carbon edge. The doping content of nitrogen element is 3at%, and the doping content of boron element is 2.8%, and the concentration of phosphoric acid element is 1.7at%. The structural representation of this material is as shown in Figure 1. Its preparation method is as follows:
A () adds mol ratio in 95 DEG C of deionized waters is the tripolycyanamide of 80:1, fructose, stirs and obtains mixed solution after being completely dissolved;
B () adds phosphoric acid in the described mixed solution of step (a), the mol ratio of phosphate radical and tripolycyanamide is 3:10, stirs to mix homogeneously rotary evaporation and dries and to obtain melamine phosphate precipitation;
C (), in tube furnace, under nitrogen protection, is warming up to 430 DEG C with 8 DEG C/min, be incubated 7 hours, be then warming up to 850 DEG C with 8 DEG C/min again, is incubated 2 hours.
Embodiment 4:
By the material made prepared by the present embodiment be intracell doped with nitrogen and boron element, then there is the grapheme material that phosphate radical and sulfate radical are modified at carbon edge. The doping content of nitrogen element is 3at%, and the doping content of boron element is 2.8%, and the concentration of phosphoric acid element is 1.7at%, and the concentration of sulfur is 2.8%. The structural representation of this material is as shown in Figure 1. Its preparation method is as follows:
A () adds mol ratio in 95 DEG C of deionized waters is the tripolycyanamide of 80:1, glucose, stirs and obtains mixed solution after being completely dissolved;
B () adds phosphoric acid and sulphuric acid in the described mixed solution of step (a), the mol ratio of phosphate radical and tripolycyanamide is 3:10, and sulfate radical and the mol ratio of tripolycyanamide are 1:2 stirring to rotary evaporation after mixing homogeneously to be dried and to obtain melamine phosphate and precipitate;
C (), in tube furnace, under nitrogen protection, is warming up to 550 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 950 DEG C with 5 DEG C/min again, is incubated 3 hours.
Claims (13)
1. a graphitized carbon material, it is characterised in that: the carbon intracell of described graphitized carbon material is embedded with nitrogen-atoms; Carbon lattice fringe is modified with the oxygen-containing functional group of phosphorus and/or element sulphur.
2. graphitized carbon material as claimed in claim 1, it is characterised in that: the carbon intracell of described graphitized carbon material is also embedded with boron atom.
3. graphitized carbon material as described in as arbitrary in claim 1-2, it is characterised in that: the oxygen-containing functional group of described phosphorus and/or element sulphur is one or more in phosphate groups, polyphosphoric acid foundation group, sulfonate group.
4. graphitized carbon material as claimed in claim 1, it is characterised in that: described nitrogen-atoms atomic percentage conc in described graphitized carbon material is 0.05-15%; In described phosphorus and/or element sulphur functional group, phosphorus and/or sulphur atom atomic percentage conc in described graphitized carbon material are 0.01-10%.
5. graphitized carbon material as claimed in claim 2, it is characterised in that: described boron atom atomic percentage conc in described graphitized carbon material is 0.01-10%; In described phosphorus and/or element sulphur functional group, phosphorus and/or sulphur atom atomic percentage conc in described graphitized carbon material are 0.01-10%.
6. the preparation method of a claim 1, the arbitrary described graphitized carbon material of 3-4: it is characterized in that: comprise the following steps,
A tripolycyanamide is mixed by () Yu Shuizhong with solubility carbon source, be simultaneously introduced acid source and stir to complete dissolve after rotary evaporation dry to obtain precipitate;
Described acid source is one or more in sulphuric acid, sulphuric acid anhydride, phosphoric acid, polyphosphoric acids, polyphosphoric acids anhydride or phosphoric acid anhydride;
B step (a) gained precipitate high-temperature process in inert atmosphere is obtained carbon intracell and is embedded with nitrogen-atoms by (), carbon lattice fringe is modified with phosphorus and/or the graphitized carbon material of element sulphur functional group.
7. the preparation method of the arbitrary described graphitized carbon material of claim 2 or 5: it is characterized in that: comprise the following steps,
A tripolycyanamide is mixed by () Yu Shuizhong with solubility carbon source, be simultaneously introduced boron source and acid source and stir to complete dissolve after rotary evaporation dry to obtain precipitate;
Described boron source is one or both in boric acid or boric acid anhydride, and acid source is one or more in sulphuric acid, sulphuric acid anhydride, phosphoric acid, polyphosphoric acids, polyphosphoric acids anhydride or phosphoric acid anhydride;
B step (a) gained precipitate high-temperature process in inert atmosphere is obtained carbon intracell and is embedded with nitrogen and boron atom by (), carbon lattice fringe is modified with phosphorus and/or the graphitized carbon material of element sulphur functional group.
8. the preparation method of graphitized carbon material as described in as arbitrary in claim 6-7, it is characterised in that: in described step (a), solubility carbon source is the one or more kinds of mixture in glucose, sucrose, fructose, maltose, lactose, crystal sugar, chitosan, polyvinyl alcohol, Polyethylene Glycol, soluble starch.
9. the preparation method of graphitized carbon material as described in as arbitrary in claim 6-7, it is characterised in that: in described step (b), inert atmosphere is one or more in nitrogen, argon or helium.
10. the preparation method of graphitized carbon material as described in as arbitrary in claim 6-7, it is characterized in that: in described step (b), the condition of high-temperature process for heating to 350-650 DEG C with 1-20 DEG C/min programming rate from room temperature, it is incubated 1-24 hour, then heat to 750-1100 DEG C with 1-20 DEG C/min programming rate, be incubated 1-24 hour.
11. the preparation method of graphitized carbon material as described in as arbitrary in claim 6-7, it is characterised in that: in described step (b), phosphorus and/or element sulphur functional group are one or more in phosphate groups, sulfonate group, polyphosphoric acid foundation group.
12. the preparation method of graphitized carbon material as described in as arbitrary in claim 6-7, it is characterized in that: in described step (a), the mol ratio of solubility carbon source and tripolycyanamide is 1:10-1:100, and the mol ratio of described acid source and tripolycyanamide is at 1:0.1-1:10; The mol ratio of boron source and tripolycyanamide is 1:0.1-1:10, tripolycyanamide mass concentration 0.1gml in water-1-1gml-1��
13. the application of graphitized carbon material as described in as arbitrary in claim 1-5, it is characterized in that: described this material has good parents' performance (hydrophilic and oleophylic), chemical stability and electric conductivity, has potential using value as electrode materials such as eelctro-catalyst, super capacitor material or lithium ion battery electrode materials.
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| CN107394136A (en) * | 2017-06-27 | 2017-11-24 | 东莞理工学院 | Carbon carrier, its preparation method and the application in lithium-sulfur cell |
| CN107394205A (en) * | 2017-03-29 | 2017-11-24 | 柯良节 | Balanced type multiphase graphene-structured battery, its manufacture method and application |
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| CN106654305A (en) * | 2016-10-21 | 2017-05-10 | 成都新柯力化工科技有限公司 | Graphene composite catalyst for fuel cell and preparation method of graphene composite catalyst |
| CN108178156B (en) * | 2016-12-08 | 2021-04-13 | 中国科学院大连化学物理研究所 | High-graphitization activated carbon electrode material and preparation and application thereof |
| CN108178156A (en) * | 2016-12-08 | 2018-06-19 | 中国科学院大连化学物理研究所 | A kind of high graphitization active carbon electrode material and its preparation and application |
| WO2018115208A1 (en) * | 2016-12-22 | 2018-06-28 | Universite De Poitiers | Method for doping oxidised graphene with nitrogen and phosphorus in order to obtain a supercapacitor electrode material |
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| CN107394205A (en) * | 2017-03-29 | 2017-11-24 | 柯良节 | Balanced type multiphase graphene-structured battery, its manufacture method and application |
| CN110691754B (en) * | 2017-05-31 | 2023-08-22 | 氢能动力公司(H2M) | Hydrogen storage product and method for preparing same |
| US11634321B2 (en) | 2017-05-31 | 2023-04-25 | Hydrogen In Motion Inc. (H2M) | Hydrogen storage product and method for manufacturing same |
| CN110691754A (en) * | 2017-05-31 | 2020-01-14 | 氢能动力公司(H2M) | Hydrogen storage product and method for producing the same |
| CN107394136A (en) * | 2017-06-27 | 2017-11-24 | 东莞理工学院 | Carbon carrier, its preparation method and the application in lithium-sulfur cell |
| CN108314015A (en) * | 2018-03-16 | 2018-07-24 | 江南大学 | A kind of preparation method of functionalization graphene aerogel microball |
| CN108554434B (en) * | 2018-04-16 | 2021-03-30 | 复旦大学 | Metal @ graphitized carbon/graphene composite electrocatalyst material and preparation method thereof |
| CN108554434A (en) * | 2018-04-16 | 2018-09-21 | 复旦大学 | Metal@graphitized carbons/graphene complex electrocatalyst materials and preparation method thereof |
| CN112366316A (en) * | 2020-09-27 | 2021-02-12 | 泰山学院 | Preparation method and application of nitrogen and phosphorus co-doped graphene |
| CN112366316B (en) * | 2020-09-27 | 2022-03-01 | 泰山学院 | Preparation method and application of nitrogen and phosphorus co-doped graphene |
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