CN105621406A - Nitrogen-doped porous graphite and preparation method thereof - Google Patents
Nitrogen-doped porous graphite and preparation method thereof Download PDFInfo
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- CN105621406A CN105621406A CN201610112736.7A CN201610112736A CN105621406A CN 105621406 A CN105621406 A CN 105621406A CN 201610112736 A CN201610112736 A CN 201610112736A CN 105621406 A CN105621406 A CN 105621406A
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Abstract
The invention discloses nitrogen-doped porous graphite and a preparation method thereof. The preparation method comprises the following steps of conducting low temperature heat treatment on a mixed aqueous solution of nitrate and a carbon source, so that a metal oxide hard template-thin carbon layer precursor is formed; conducting graphitization on the obtained metal oxide hard template-thin carbon layer precursor, so that the nitrogen-doped porous graphite is obtained. According to the method, raw materials are conventional materials, process cost is low, and conditions of the method are easy to meet; the novel template method is adopted for directly pyrolyzing saccharides organic matter, so that the nitrogen-doped porous graphite is obtained, and the process is quite simple and fast; the nitrogen-doped porous graphite is quite simple in operation, low in cost, high in yield and capable of being produced on a large scale, the less-layer porous graphite which has abundant surface pores, narrow in pore size distribution and high in specific surface area can be obtained, and the nitrogen-doped porous graphite and the preparation method thereof are applicable to such fields as supercapacitors, fuel-cell catalysts, electrocatalysis, lithium batteries, adsorption and gas separation.
Description
Technical field
The present invention relates to technical field of nano material, specifically a kind of N doping porous graphene and preparation method thereof.
Background technology
Graphene, since being found, due to the performance that it is superior in a lot, has become study hotspot recently for over ten years. But the application of Graphene also faces all difficulties. Applying for Graphene, it is most important to the regulation and control of structure. Recently, a kind of new Graphene space structure, porous graphene is with abundant bivariate table face, material can be made quickly to transmit and effectively stop Graphene to be again piled into graphite-structure because of intermolecular force, substantial amounts of come-at-able surface defect, big specific surface area, the advantage such as abundant surface functional groups receives more concern, and it has wide practical use in fields such as ultracapacitor, fuel-cell catalyst, electro-catalysis, lithium cell cathode material, absorption, gas sensors.
The current method preparing Graphene on a large scale is mainly graphene oxide reducing process. And the preparation of porous graphene obtains with different mode etching oxidation Graphene mainly by the method for " from top to bottom ". But often there is following obvious shortcoming in these methods: complicated preparation technology, it is difficult to preparing on a large scale, relatively costly, pore-size distribution is wider, and specific surface area is less (is typically smaller than 1000m2g-1), or reunion heavy damage shortcomings such as original two-dimensional structure again. XPwang have studied the method that one " from top to bottom " prepares N doping porous graphene equal within 2016, delivering High-DensityMonolithofN-DopedHoleyGrapheneforUltrahighVo lumetricCapacityofLi-IonBatteries on AdvancedEnergyMaterials magazine, first pass through hydrogen peroxide etching oxidation Graphene and obtain porous oxidation Graphene, again through polymer, porous graphene is carried out high temperature nitrogen doping and obtain N doping porous graphene, but the N doping porous graphene pore-size distribution on its gained is wider, specific surface area only has 612m2g-1. Limited porosity and specific surface area are not sufficient to the advantage playing porous graphene greatly. Simultaneously effective N doping can also improve the performance of porous graphene, such as lithium battery and ultracapacitor in a lot. The report being directly synthesized porous graphene by " from bottom to top " method is then less.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide a kind of economy can N doping porous graphene " from bottom to top " preparation method of scale and the narrower high-specific surface area of pore-size distribution.
The present invention seeks to be achieved through the following technical solutions:
First aspect, the preparation method that the present invention provides a kind of N doping porous graphene, comprise the steps:
The mixed aqueous solution of nitrate, carbon source is carried out Low Temperature Heat Treatment, forms metal-oxide hard template-ultra-thin carbon-coating predecessor;
Gained metal-oxide hard template-ultra-thin carbon-coating predecessor is carried out graphitization, to obtain final product.
Preferably, described nitrate is zinc nitrate hexahydrate or magnesium nitrate hexahydrate; Described nitrate function as pore creating material, nitrogenous source and template predecessor.
Preferably, described carbon source is saccharide Organic substance.
It is further preferred that described saccharide Organic substance is the soluble sugar type organics such as glucose, sucrose, fructose, soluble starch.
Preferably, the mass ratio of described nitrate and carbon source is (2��4): 1. When ratio is less than 2:1, carbon-coating is thicker, and when ratio is more than 4:1, major part carbon source can be fallen by reactive ion etching.
Preferably, described Low Temperature Heat Treatment specifically carries out under air ambient.
Preferably, the temperature of described Low Temperature Heat Treatment is 150��500 DEG C.
Heretofore described Low Temperature Heat Treatment specifically carries out in Muffle furnace, until nitrate and carbon source react rapidly become metal-oxide hard template and the ultra-thin carbon-coating predecessor of porous after take out immediately.
Preferably, described graphitization is specifically by gained metal-oxide hard template-ultra-thin carbon-coating predecessor heat treatment under non-oxidizing gas atmosphere.
Preferably, described non-oxidizing gas is the mixing of one or more in nitrogen, argon.
Preferably, described heat treated temperature be 500��1700 DEG C, the time be 5��120min.
Heretofore described graphitization carries out in tube furnace.
Preferably, in described preparation method, the temperature of Low Temperature Heat Treatment is 2��30 DEG C/min to the Cooling rate of graphited temperature.
Preferably, described method also includes step that the N doping porous graphene obtained carries out pickling; The effect of described pickling is in that to remove metal-oxide.
Second aspect, the present invention provides a kind of N doping porous graphene prepared by described preparation method.
Compared with prior art, the present invention has following beneficial effect:
(1) the inventive method raw material is conventional material, and established technology cost is low, and method condition readily satisfies;
(2) the inventive method adopts " from bottom to top " method to be directly synthesized N doping porous graphene, and its technique is very simple and can have abundant surface holes, high specific surface area, narrower pore-size distribution by gained porous graphene;
(3) the inventive method time is short, and productivity is high, and operation is very simple, and cost is low, and can be mass-produced, and can obtain the N doping porous graphene of the narrower high-specific surface area of pore-size distribution, be suitable for commercially producing.
Accompanying drawing explanation
By reading detailed description non-limiting example made with reference to the following drawings, the other features, objects and advantages of the present invention will become more apparent upon:
Fig. 1 is the ultra-thin carbon-coating of the zinc oxide/porous/zinc oxide sandwich Product scan Electronic Speculum figure of the preparation of embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of N doping porous graphene prepared by embodiment 1;
Fig. 3 is the high resolution scanning Electronic Speculum figure of N doping porous graphene prepared by embodiment 1;
Fig. 4 is the isothermal adsorption desorption curve figure of N doping porous graphene prepared by embodiment 1;
Fig. 5 is the graph of pore diameter distribution of N doping porous graphene prepared by embodiment 2.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail. Following example will assist in those skilled in the art and are further appreciated by the present invention, but do not limit the present invention in any form. It should be pointed out that, to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement. These broadly fall into protection scope of the present invention.
Embodiment 1
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Zinc nitrate hexahydrate and glucose example 4:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 150 DEG C fast reaction formed the ultra-thin carbon-coating of zinc oxide/porous/zinc oxide sandwich product, scanning electron microscope (SEM) photograph is as shown in Figure 1;
Then by ultra-thin for zinc oxide/porous carbon-coating/zinc oxide sandwich product further in tube furnace, heating rate is 10 DEG C/min, it is heated at 800 DEG C under non-oxidizing gas atmosphere and is incubated after the further graphitization of 5min, wash away zinc oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 2��6nm, and specific surface area is 1602m2g-1, nitrogen element content is 7.35%, and productivity is approximately about 3%, and its scanning electron microscope (SEM) photograph, high resolution scanning Electronic Speculum figure, isothermal adsorption desorption curve figure, graph of pore diameter distribution are respectively as shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5. Ultra-thin carbon-coating surface has been covered with nano level ZnO particle as seen from Figure 1. Fig. 2 shows the structure of typical Graphene fold. Fig. 3 position porous graphene high-resolution SEM photograph, hence it is evident that see that surface exists large number of orifices. From Fig. 5, the pore-size distribution of sample can significantly see that the pore size in graphenic surface hole is mainly within the scope of 2��6nm.
Embodiment 2
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Zinc nitrate hexahydrate and soluble starch example 4:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 150 DEG C fast reaction form the ultra-thin carbon-coating of zinc oxide/porous/zinc oxide sandwich product;
Then by ultra-thin for zinc oxide/porous carbon-coating/zinc oxide sandwich product further in tube furnace, heating rate is 30 DEG C/min, is heated to 500 DEG C of insulation 120min, after further graphitization under non-oxidizing gas atmosphere, zinc oxide is washed away with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 2��6nm, and Fig. 5 is shown in by pore-size distribution.
Embodiment 3
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Zinc nitrate hexahydrate and sucrose example 4:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 500 DEG C fast reaction form the ultra-thin carbon-coating of zinc oxide/porous/zinc oxide sandwich product;
Then by ultra-thin for zinc oxide/porous carbon-coating/zinc oxide sandwich product further in tube furnace, heating rate is 2 DEG C/min, it is heated at 1700 DEG C under non-oxidizing gas atmosphere and is incubated after the further graphitization of 5min, wash away zinc oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 2��6nm.
Embodiment 4
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Magnesium nitrate hexahydrate and glucose example 2:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 150 DEG C fast reaction form the ultra-thin carbon-coating of magnesium oxide/porous/magnesium oxide sandwich product;
Then by ultra-thin for magnesium oxide/porous carbon-coating/magnesium oxide sandwich product further in tube furnace, heating rate is 10 DEG C/min, it is heated at 1700 DEG C under non-oxidizing gas atmosphere and is incubated after the further graphitization of 5min, wash away magnesium oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 1��4nm.
Embodiment 5
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Magnesium nitrate hexahydrate and fructose example 3:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 220 DEG C fast reaction form the ultra-thin carbon-coating of magnesium oxide/porous/magnesium oxide sandwich product;
Then by ultra-thin for magnesium oxide/porous carbon-coating/magnesium oxide sandwich product further in tube furnace, heating rate is 2 DEG C/min, it is heated at 500 DEG C under high pure nitrogen atmosphere and is incubated after the further graphitization of 120min, wash away magnesium oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 1��4nm. Productivity is approximately about 7%.
Embodiment 6
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Magnesium nitrate hexahydrate and fructose example 3:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 500 DEG C fast reaction form the ultra-thin carbon-coating of magnesium oxide/porous/magnesium oxide sandwich product;
Then by ultra-thin for magnesium oxide/porous carbon-coating/magnesium oxide sandwich product further in tube furnace, heating rate is 30 DEG C/min, it is heated at 500 DEG C under high-purity argon gas atmosphere atmosphere and keeps after the further graphitization of 120min, wash away magnesium oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 1��4/nm.
Embodiment 7
The present embodiment relate to a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution, described method comprises the steps:
Magnesium nitrate hexahydrate and starch example 3:1 in mass ratio are dissolved in aqueous, by mixed aqueous solution first under Muffle furnace air ambient at 150 DEG C fast reaction form the ultra-thin carbon-coating of magnesium oxide/porous/magnesium oxide sandwich product;
Then by ultra-thin for magnesium oxide/porous carbon-coating/magnesium oxide sandwich product further in tube furnace, heating rate is 10 DEG C/min, it is heated at 1100 DEG C under the atmosphere of high pure nitrogen and argon mixing after the maintenance further graphitization of 5min, washes away magnesium oxide with aqueous acid.
N doping porous graphene data analysis prepared by the present embodiment is known: pore diameter range is 1��4nm.
Comparative example 1
This comparative example is the comparative example of embodiment 1, and contrast part is only that, zinc nitrate hexahydrate and glucose example 4.5:1 in mass ratio;
By analysis, the products collection efficiency that this comparative example prepares is very low, and lower than 0.5%, oxidized dose of most carbon source reacts into gas.
Comparative example 2
This comparative example is the comparative example of embodiment 1, and contrast part is only that, zinc nitrate hexahydrate and glucose example 1.5:1 in mass ratio;
By analysis, the product carbon layers having thicknesses that this comparative example prepares is blocked up, it is difficult to graphitization, and specific surface area is less.
In sum; the invention provides a kind of economy can the N doping porous graphene preparation method of scale and the narrower high-specific surface area of pore-size distribution; achieve the preparation technology time short; productivity is high; simple to operate, cost is low, and the purpose that can be mass-produced; the more important thing is, prepare gained porous graphene and there is abundant surface holes, high specific surface area, narrower pore-size distribution.
Above specific embodiments of the invention are described. It is to be appreciated that the invention is not limited in above-mentioned particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, and this has no effect on the flesh and blood of the present invention.
Claims (10)
1. the preparation method of a N doping porous graphene, it is characterised in that comprise the steps:
The mixed aqueous solution of nitrate, carbon source is carried out Low Temperature Heat Treatment, forms metal-oxide hard template-ultra-thin carbon-coating predecessor;
Gained metal-oxide hard template-thin carbon layer predecessor is carried out graphitization, to obtain final product.
2. the preparation method of N doping porous graphene according to claim 1, it is characterised in that described nitrate is one or both in zinc nitrate hexahydrate, magnesium nitrate hexahydrate.
3. the preparation method of N doping porous graphene according to claim 1, it is characterised in that described carbon source is saccharide Organic substance.
4. the preparation method of N doping porous graphene according to claim 1, it is characterised in that the mass ratio of described nitrate and carbon source is (2��4): 1.
5. the preparation method of N doping porous graphene according to claim 1, it is characterised in that described Low Temperature Heat Treatment specifically carries out under air ambient; The temperature of described Low Temperature Heat Treatment is 150��500 DEG C.
6. the preparation method of N doping porous graphene according to claim 1, it is characterised in that described graphitization is the heat treatment under non-oxidizing gas atmosphere by gained metal-oxide hard template and ultra-thin carbon-coating predecessor specifically.
7. the preparation method of N doping porous graphene according to claim 6, it is characterised in that described non-oxidizing gas is the mixing of one or more in nitrogen, argon; Described heat treated temperature is 500��1700 DEG C, the time is 5��120min.
8. the preparation method of N doping porous graphene according to claim 1, it is characterised in that in described preparation method, the temperature of Low Temperature Heat Treatment is 2��30 DEG C/min to the Cooling rate of graphited temperature.
9. the preparation method of N doping porous graphene according to claim 1, it is characterised in that described method also includes the step that the N doping porous graphene obtained carries out pickling.
10. a N doping porous graphene, it is characterised in that can be prepared by the arbitrary preparation method of claim 1 to 9.
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| CN106219521A (en) * | 2016-07-12 | 2016-12-14 | 昆明理工大学 | A kind of preparation method of three-dimensional foam Graphene |
| CN106587017A (en) * | 2016-12-14 | 2017-04-26 | 中国石油大学(北京) | Porous graphene and preparation method thereof |
| CN107140623A (en) * | 2017-05-24 | 2017-09-08 | 郑州大学 | A kind of method for preparing graphene |
| CN107619040A (en) * | 2017-11-01 | 2018-01-23 | 中国科学院兰州化学物理研究所 | The method that partial combustion method quickly prepares porous graphene |
| CN109473684A (en) * | 2018-09-29 | 2019-03-15 | 中国科学院山西煤炭化学研究所 | The elctro-catalyst and preparation method of a kind of sulphur-nitrogen-carbon-based oxygen reduction of transition metal codope and application |
| CN109678139A (en) * | 2017-10-18 | 2019-04-26 | 天津大学 | Fluorine nitrogen codope porous graphene hydrogel and preparation method thereof for electrode of super capacitor |
| CN110858523A (en) * | 2018-08-22 | 2020-03-03 | 北京纳米能源与***研究所 | Manufacturing method of super capacitor |
| CN111924822A (en) * | 2020-07-27 | 2020-11-13 | 山东理工大学 | Preparation method of low-frequency efficient wave-absorbing SiC/porous carbon composite material |
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| CN106219521A (en) * | 2016-07-12 | 2016-12-14 | 昆明理工大学 | A kind of preparation method of three-dimensional foam Graphene |
| CN106219521B (en) * | 2016-07-12 | 2018-08-31 | 昆明理工大学 | A kind of preparation method of three-dimensional foam graphene |
| CN106587017A (en) * | 2016-12-14 | 2017-04-26 | 中国石油大学(北京) | Porous graphene and preparation method thereof |
| CN107140623A (en) * | 2017-05-24 | 2017-09-08 | 郑州大学 | A kind of method for preparing graphene |
| CN109678139A (en) * | 2017-10-18 | 2019-04-26 | 天津大学 | Fluorine nitrogen codope porous graphene hydrogel and preparation method thereof for electrode of super capacitor |
| CN107619040A (en) * | 2017-11-01 | 2018-01-23 | 中国科学院兰州化学物理研究所 | The method that partial combustion method quickly prepares porous graphene |
| CN107619040B (en) * | 2017-11-01 | 2019-11-19 | 中国科学院兰州化学物理研究所 | The method that partial combustion method quickly prepares porous graphene |
| CN110858523A (en) * | 2018-08-22 | 2020-03-03 | 北京纳米能源与***研究所 | Manufacturing method of super capacitor |
| CN110858523B (en) * | 2018-08-22 | 2022-07-08 | 北京纳米能源与***研究所 | Manufacturing method of super capacitor |
| CN109473684A (en) * | 2018-09-29 | 2019-03-15 | 中国科学院山西煤炭化学研究所 | The elctro-catalyst and preparation method of a kind of sulphur-nitrogen-carbon-based oxygen reduction of transition metal codope and application |
| CN111924822A (en) * | 2020-07-27 | 2020-11-13 | 山东理工大学 | Preparation method of low-frequency efficient wave-absorbing SiC/porous carbon composite material |
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