CN108101037B - A kind of preparation method of nitrogen-doped graphene material based on diaminoazofurazan - Google Patents
A kind of preparation method of nitrogen-doped graphene material based on diaminoazofurazan Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 42
- YBRXRTHOHUWQLL-UHFFFAOYSA-N 4-[(4-amino-1,2,5-oxadiazol-3-yl)diazenyl]-1,2,5-oxadiazol-3-amine Chemical compound NC1=NON=C1N=NC1=NON=C1N YBRXRTHOHUWQLL-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000005496 eutectics Effects 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- XEUSVFYYNLXDNL-UHFFFAOYSA-N bis(1,2,5-oxadiazol-3-yl)diazene Chemical compound C1=NON=C1N=NC1=NON=C1 XEUSVFYYNLXDNL-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- SQVRNJKIWUCVCY-UHFFFAOYSA-N 4-(1,2,5-oxadiazol-3-yldiazenyl)-1,2,5-oxadiazol-3-amine Chemical compound C1=NON=C1N=NC2=NON=C2N SQVRNJKIWUCVCY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000654 additive Substances 0.000 abstract 1
- -1 diaminoazofurazan ethanol Chemical compound 0.000 abstract 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- ILVXOBCQQYKLDS-UHFFFAOYSA-N pyridine N-oxide Chemical compound [O-][N+]1=CC=CC=C1 ILVXOBCQQYKLDS-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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Abstract
本发明实施例提供一种基于二氨基偶氮呋咱的氮掺杂石墨烯材料的制备方法，涉及材料制备技术领域。其中，该方法包括：将石墨烯分散于水中，加入二氨基偶氮呋咱乙醇溶液，在50～70℃下加热30～60min，降温至20～40℃，干燥，得到石墨烯包覆的二氨基偶氮呋咱共晶物，其中，石墨烯与二氨基偶氮呋咱溶液中的二氨基偶氮呋咱的质量比为1:1～10，将二氨基偶氮呋咱共晶物研磨成粉末，在500～800℃下加热3～5h，得到氮掺杂石墨烯材料。利用二氨基偶氮呋咱与石墨烯进行反应，得到氮掺杂含量较高的石墨烯材料。该材料中石墨烯均匀包覆在DAAF晶体的表面，不需要使用胶黏剂等助剂，完整的保持了二氨基偶氮呋咱晶体的表面性能。
The embodiment of the present invention provides a method for preparing a nitrogen-doped graphene material based on diaminoazofurazan, which relates to the technical field of material preparation. Wherein, the method comprises: dispersing graphene in water, adding diaminoazofurazan ethanol solution, heating at 50-70° C. for 30-60 min, cooling to 20-40° C., and drying to obtain graphene-coated graphene Aminoazofurazan eutectic, wherein the mass ratio of graphene to diaminoazofurazan solution in diaminoazofurazan solution is 1:1-10, and the diaminoazofurazan eutectic is ground powder, and heated at 500-800° C. for 3-5 hours to obtain nitrogen-doped graphene material. Diaminoazofurazan is used to react with graphene to obtain graphene material with high nitrogen doping content. In this material, graphene is evenly coated on the surface of the DAAF crystal, without the use of adhesives and other additives, and the surface properties of the diaminoazofurazan crystal are completely maintained.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a method for preparing a nitrogen-doped graphene material based on diamino azo furazan.
Background
Graphene (G) is a two-dimensional honeycomb lattice material formed by closely bonding planar single-layer carbon atoms, has a thickness of about 0.35 nm, and is the thinnest two-dimensional material in the world.
The electrons of the graphene pass through the graphene without any resistance, the generated heat is less, the conductive efficiency is high, the graphene is the material with the best known conductive performance, and the graphene has unique performance, for example, the tensile strength can reach 130 GPa; the carrier mobility can reach 15000-2Vs (square centimeter per volt-second), which can be more than 10 times that of a silicon wafer; the thermal conductivity can reach 5000W/mK (watt per milli heat conductivity coefficient), which is 3 times of that of diamond; it also has the special properties of room-temperature quantum Hall effect and room-temperature ferromagnetism.
However, graphene has no band gap, its conductivity cannot be controlled as in a conventional semiconductor, and its surface is smooth and inert, which is not conducive to compounding with other materials. The above disadvantages limit the applications of graphene.
Disclosure of Invention
The invention provides a preparation method of a nitrogen-doped graphene material based on diamino azo furazan, and aims to solve the problem that the application of the graphene material is limited due to the fact that the graphene material is not easy to be compounded with other materials.
The invention provides a preparation method of a nitrogen-doped graphene material based on diamino azo furazan, which comprises the following steps:
dispersing graphene in water, adding a diamino azofurazan solution, heating at 50-70 ℃ for 30-60 min, cooling to 20-40 ℃, and drying to obtain a graphene-coated diamino azofurazan eutectic crystal; the mass ratio of the graphene to the diamino azo furazan in the diamino azo furazan solution is 1: 1-10;
grinding the diamino azo furazan eutectic compound into powder, and heating for 3-5 h at 500-800 ℃ to obtain the nitrogen-doped graphene material.
According to the preparation method of the nitrogen-doped graphene material, provided by the invention, diaminoazofurazan is used for reacting with graphene to obtain the graphene material with high nitrogen doping content. In the material, graphene is uniformly coated on the surface of the diamino azo furazan crystal, auxiliaries such as an adhesive are not needed, and the surface performance of the diamino azo furazan crystal is completely maintained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention.
FIG. 1 is a schematic flow chart of a preparation method of a nitrogen-doped graphene material based on diaminoazofurazan, provided by an embodiment of the invention;
fig. 2 is a scanning electron microscope test chart of the nitrogen-doped graphene material prepared in example 1 of the present invention;
FIG. 3 is an X-ray photoelectron spectroscopy test chart of the nitrogen-doped graphene material prepared in example 1 of the present invention;
fig. 4 is an X-ray photoelectron spectroscopy test chart of the nitrogen-doped graphene material N1s prepared in example 1 of the present invention;
fig. 5 is an X-ray photoelectron spectroscopy test chart of C1s of the nitrogen-doped graphene material prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, fig. 1 is a schematic flow chart of a method for preparing a nitrogen-doped graphene material based on diaminoazofurazan according to an embodiment of the present invention, where the method includes:
dispersing graphene in water, adding a diamino azofurazan (DAAF) solution, heating at 50-70 ℃ for 30-60 min, cooling to 20-40 ℃, and drying to obtain a graphene-coated DAAF eutectic compound;
wherein the mass ratio of the graphene to the DAAF is 1: 1-10;
and step two, grinding the DAAF eutectic into powder, and heating for 3-5 hours at 500-800 ℃ to obtain the nitrogen-doped graphene material.
According to the preparation method of the nitrogen-doped graphene material, provided by the invention, DAAF is reacted with graphene to obtain the graphene material with high nitrogen doping content. In the material, graphene is uniformly coated on the surface of the DAAF crystal, auxiliaries such as an adhesive are not needed, and the surface performance of the diaminoazofurazan crystal is completely maintained. Furthermore, the material opens the energy band gap, adjusts the conductivity type and changes the electronic structure; the density of free carriers is improved, and the conductivity and stability are improved; the introduction of the functional group containing nitrogen increases the active sites of the metal particles adsorbed on the surface, enhances the interaction between the metal particles and the graphene, and expands the application of the graphene.
In the first step of the method,
specifically, the graphene has 1 to 3 layers and a sheet diameter of 0.2 to 100 μm. Deionized water is selected and mixed with graphene. The DAAF solution is a mixed solution of DAAF and ethanol, wherein the concentration of the DAAF is 1-5 mg/mL.
Further, after dispersing graphene in water, stirring for 30-90 min by using a magnetic stirrer, placing in an ultrasonic disperser, and ultrasonically shaking for 30-60 min. The mass ratio of the graphene to the deionized water is 1: 20-30.
Specifically, the DAAF solution is a mixed solution of DAAF and ethanol, wherein the concentration of the DAAF is 1-5 mg/mL. Preferably, the concentration of the DAAF solution is 3 mg/L. The mass ratio of the graphene to the DAAF in the DAAF solution is 1: 1-10, preferably 1: 4-8, and more preferably 1: 8.
In the second step, the first step is carried out,
preferably, the heating temperature of the DAAF eutectic compound is 600 ℃ and the heating time is 4 h.
Example 1
Adding 0.1 g of graphene with the sheet diameter of 0.2 mu m into 25ml of deionized water, magnetically stirring for 60 minutes at the rotating speed of 600 r/min, and then placing the graphene in an ultrasonic dispersion instrument for ultrasonic treatment for 60 minutes to obtain a graphene solution with the concentration of 4 mg/ml.
And (3) melting 0.8 g of DAAF into 25ml of ethanol, adding the graphene solution, heating at 50 ℃ for 30 min, cooling to 20 ℃, and drying for 48h to obtain the graphene-coated DAAF eutectic crystal.
Grinding the DAAF eutectic crystal into powder, placing the powder in a tube furnace, heating the powder to 500 ℃, and preserving heat for 3 hours to obtain the nitrogen-doped graphene material with the nitrogen content of 5.16%.
Example 2
Adding 0.1 g of graphene with the sheet diameter of 100 mu m into 25ml of deionized water, magnetically stirring for 60 minutes at the rotating speed of 600 r/min, and then placing the graphene in an ultrasonic dispersion instrument for ultrasonic treatment for 30 minutes to obtain a graphene solution with the concentration of 4 mg/ml.
And (3) melting 0.4g of DAAF into 25ml of ethanol, adding the graphene solution, heating at 70 ℃ for 60min, cooling to 40 ℃, and drying for 48h to obtain the graphene-coated DAAF eutectic compound.
Grinding the DAAF eutectic crystal into powder, placing the powder in a tube furnace, heating to 800 ℃, and preserving heat for 5 hours to obtain the nitrogen-doped graphene material with the nitrogen content of 4.29%.
SEM (scanning electron microscope) tests were performed on the nitrogen-doped graphene material prepared in example 1, as shown in fig. 2, and fig. 2 shows SEM test images of the nitrogen-doped graphene material prepared in example 1. As shown in figure 2, graphene in the material is uniformly coated on the surface of the DAAF crystal, auxiliaries such as an adhesive are not needed, and the surface performance of the diaminoazofurazan crystal is completely maintained.
The nitrogen-doped graphene material and the non-nitrogen-doped graphene material prepared in example 1 were subjected to an X-ray photoelectron spectroscopy (XPS) test. As shown in fig. 3, it can be seen from fig. 3 that a peak appears in the binding energy at 398-.
Further, XPS analysis of N1s of nitrogen-doped graphene showed that pyridine type N, pyrrole type N, graphite type N, and pyridine N oxide appeared at 398.4, 400.1, 401.2, and 402.4 eV, respectively, as shown in fig. 4.
Further, XPS analysis at C1s of nitrogen-doped graphene showed that C-C, C-N, C-O and C = O (C = N) bonds appeared at 284.4, 285.2, 286.4 and 289.2 eV, respectively, as shown in fig. 4, indicating that DAAF as a nitrogen source for preparing nitrogen-doped graphene acted on the mechanism of graphene.
Combining the above tests, it is demonstrated that DAAF as a nitrogen source doped with graphene is feasible.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A preparation method of nitrogen-doped graphene material based on diamino azo furazan is characterized by comprising the following steps:
dispersing graphene in water, adding a diamino azofurazan ethanol solution, heating at 50-70 ℃ for 30-60 min, cooling to 20-40 ℃, and drying to obtain a graphene-coated diamino azofurazan eutectic crystal; the mass ratio of the graphene to the diamino azo furazan in the diamino azo furazan solution is 1: 1-10;
grinding the diamino azo furazan eutectic compound into powder, and heating for 3-5 h at 500-800 ℃ to obtain the nitrogen-doped graphene material.
2. The method according to claim 1, wherein the number of graphene layers is 1-3, and the sheet diameter is 0.2-100 μm.
3. The method according to claim 1, wherein the mass ratio of the graphene to the diaminoazofurazan is 1: 4-8.
4. The method according to claim 1, wherein the diaminoazofurazan solution is a mixed solution of diaminoazofurazan and ethanol, and the concentration of the diaminoazofurazan is 1-5 mg/mL.
5. The method according to claim 1, wherein the heating temperature of the diaminoazofurazan eutectic compound is 600 ℃.
6. The method according to claim 1, characterized in that the heating time of the diaminoazofurazan eutectic compound is 4 h.
7. The method of claim 1, further comprising:
adding the graphene into deionized water, stirring for 30-90 min, and ultrasonically shaking for 30-60 min, wherein the mass ratio of the graphene to the deionized water is 1: 20-30.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019119459A1 (en) * | 2017-12-23 | 2019-06-27 | 深圳大学 | Diamino azofurazan-based method for preparing nitrogen-doped graphene material |
| WO2019119460A1 (en) * | 2017-12-23 | 2019-06-27 | 深圳大学 | Method for preparing nitrogen-doped graphene from furazan derivatives as nitrogen source |
| CN109776444A (en) * | 2019-03-11 | 2019-05-21 | 中国工程物理研究院化工材料研究所 | Method based on natural subsidence process preparation high dispersive DAAF nano-powder |
| CN110980716A (en) * | 2019-12-26 | 2020-04-10 | 广东石油化工学院 | A kind of preparation method of nitrogen-doped graphene material based on 4-amino-1,2,4-triazole |
| CN110980714A (en) * | 2019-12-26 | 2020-04-10 | 广东石油化工学院 | A kind of preparation method of nitrogen-doped graphene material based on 4,4'-azo-1,2,4-triazole |
| CN111017917A (en) * | 2019-12-26 | 2020-04-17 | 广东石油化工学院 | A kind of preparation method of nitrogen-doped graphene material based on 4-amino-1,2,4-triazol-5-one |
| CN110980715A (en) * | 2019-12-26 | 2020-04-10 | 广东石油化工学院 | A kind of preparation method of nitrogen-cobalt co-doped graphene material based on 4-amino-1,2,4-triazol-5-one cobalt salt |
| CN111072021A (en) * | 2019-12-26 | 2020-04-28 | 广东石油化工学院 | Preparation method of nitrogen-doped graphene material based on 5,5 '-diamino-3, 3' -1,2, 4-triazole |
| CN110937597A (en) * | 2019-12-26 | 2020-03-31 | 广东石油化工学院 | A kind of preparation method of nitrogen-doped graphene material based on 3,5-diamino-1 hydrogen-1,2,4-triazole |
| CN110980713A (en) * | 2019-12-26 | 2020-04-10 | 广东石油化工学院 | A kind of preparation method of graphene material based on 5,5'-diamino-3,3'-1,2,4-triazole cobalt salt |
| CN111003707A (en) * | 2019-12-26 | 2020-04-14 | 广东石油化工学院 | Preparation method of nitrogen-doped graphene material based on 4, 4' -azo-1, 2, 4-triazole-5-ketone |
| CN116375598B (en) * | 2023-03-29 | 2024-09-13 | 吉林医药学院 | 4,4' -Azo dibenzoate phenanthroline dye eutectic and preparation method thereof |
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| CN103803539A (en) * | 2014-02-17 | 2014-05-21 | 上海交通大学 | Nitrogen-doped graphene oxide material and preparation method thereof |
| CN104229781A (en) * | 2014-09-09 | 2014-12-24 | 东莞市翔丰华电池材料有限公司 | Method for preparing nitrogen-doped graphene with high nitrogen doping amount |
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| CN103803539A (en) * | 2014-02-17 | 2014-05-21 | 上海交通大学 | Nitrogen-doped graphene oxide material and preparation method thereof |
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