CN103449411A - Preparation method for nitrogen-doped graphene - Google Patents
Preparation method for nitrogen-doped graphene Download PDFInfo
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- CN103449411A CN103449411A CN2012101738659A CN201210173865A CN103449411A CN 103449411 A CN103449411 A CN 103449411A CN 2012101738659 A CN2012101738659 A CN 2012101738659A CN 201210173865 A CN201210173865 A CN 201210173865A CN 103449411 A CN103449411 A CN 103449411A
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Abstract
The invention provides a preparation method for nitrogen-doped graphene. The preparation method comprises the following steps: taking a pore forming agent and graphite oxide according to a mass ratio of 0.01-0.5:1 for mixing, then dissolving in water, and carrying out ultrasonic treatment for 30-60 minutes to obtain a mixed solution with the concentration of 0.1-10 g/L; then filtering, collecting a filtered matter, and carrying out drying treatment of the filtered matter to obtain a powder; and under the protection of inert gas, placing the dried powder at a temperature of 500-580 DEG C to carry out reduction treatment for 1-30 min, followed by stopping heating, naturally cooling to the room temperature, stopping introducing the inert gas, and thereby obtaining the nitrogen-doped graphene. The method has wide sources of the raw materials, low cost, and easy and convenient operation, has no special requirements on equipment, and is liable to mass production.
Description
Technical field
The present invention relates to the synthetic field of material, particularly relate to a kind of preparation method of nitrating Graphene.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal that the strong K of the peace moral of Univ Manchester UK in 2004 sea nurse (Andre K.Geim) etc. is found, is the carbon material as thin as a wafer of single or multiple lift.Single-layer graphene has good conduction, heat conductivility and low thermal expansivity, and its theoretical specific surface area is up to 2630m
2/ g (A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), can be used for effect transistor, electrode materials, matrix material, liquid crystal display material, sensor.
The method for preparing at present Graphene mainly contain graphite breakaway (et al.Science 2004,306,666 for Novoselov K S, Geim A K), chemistry redox method [D A Dikin, et al.Nature 2007,448,457; Sasha Stankovich, Dmitriy A Dikin, Richard D Piner, et al.Carbon 2007,45,1558], ultrasonic stripping method (Guohua Chen, Wengui Weng, Dajun Wu, et al.Carbon.2004,42,753), chemical Vapor deposition process (Alexander N, Obraztsov.Nature nanotechnology.2009,4,212) etc.Usually, the Graphene that prepared by these methods is all the Graphene of intrinsic.
Theoretical investigation shows, Graphene energy band structure after the nitrogen doping has adjustment, thereby can greatly expand the application of Graphene in fields such as optics, electricity and magnetics.At present, the preparation method of disclosed nitrating Graphene is mainly chemical Vapor deposition process and electrochemical process.In chemical Vapor deposition process, depositing time is the key of controlling synthesizing graphite alkene, and prepared Graphene product is the film graphene film.The nitrating Graphene of electrochemical production, the nitrogen element all is present in the edge of graphene sheet layer, does not enter in graphene sheet layer, and the method preparation process is comparatively complicated in addition.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of preparation method of nitrating Graphene, nitrogen-doping is entered in graphene sheet layer to the nitrating Graphene that makes vesicular structure.The method raw material sources are wide, cost is low, simple to operation, and equipment, without particular requirement, is easy to mass and produces.
The invention provides a kind of preparation method of nitrating Graphene, comprise the following steps:
The ratio that to get pore-forming material be 0.01～0.5: 1 with graphite oxide in mass ratio is soluble in water after mixing, and supersound process 30～60 minutes, make the mixing solutions that concentration is 0.1～10g/L; Then filter, collect screening and screening is carried out to drying treatment, make powder;
Under protection of inert gas, described dried powder is placed at 500～580 ℃ of temperature to reduce and processes 1～30 minute, stop subsequently heating, naturally cool to room temperature, stop passing into rare gas element, obtain the nitrating Graphene.
Preferably, pore-forming material is a kind of or its arbitrary combination in volatile salt, bicarbonate of ammonia, ammonium nitrate, ammonium sulfate, monoammonium sulfate, ammonium sulphite, ammonium chloride.
In the supersound process process, graphite oxide is by the ultrasonic graphene oxide that is dispersed into, and simultaneously, inorganic nitrogenous substances obtains mixing uniformly fully with graphene oxide.
Preferably, the temperature of drying treatment is 40～60 ℃, and be 24～48h time of drying.
In the reduction reaction process, under the effect of high temperature, the functional group on graphene oxide surface decomposes generation CO
2deng gas, gas produces abundant hole after overflowing on graphene oxide, simultaneously, inorganic nitrogenous substances is decomposes effusion nitrogenous gas also, also produce pore space structure on inorganic nitrogenous substances, and the nitrogenous gas of overflowing enters doping in the defective graphene sheet layer of self tool, make the nitrating Graphene.
Preferably, reduction reaction is carried out in high temperature process furnances.
Preferably, rare gas element is argon gas, nitrogen or helium, or the mixed gas of any two kinds in argon gas, nitrogen and helium.
The preparation method of a kind of nitrating Graphene provided by the invention, enter nitrogen-doping in graphene sheet layer the nitrating Graphene that makes vesicular structure.These preparation method's raw material sources are wide, cost is low, simple to operation, and equipment, without particular requirement, is easy to mass and produces.
The accompanying drawing explanation
Fig. 1 is the prepared Graphene SEM figure of the embodiment of the present invention one.
Embodiment
The invention provides a kind of preparation method of nitrating Graphene, comprise the following steps:
The ratio that to get pore-forming material be 0.01～0.5: 1 with graphite oxide in mass ratio is soluble in water after mixing, and supersound process 30～60 minutes, make the mixing solutions that concentration is 0.1～10g/L; Then filter, collect screening and screening is carried out to drying treatment, make powder;
Under protection of inert gas, described dried powder is placed at 500～580 ℃ of temperature to reduce and processes 1～30 minute, stop subsequently heating, naturally cool to room temperature, stop passing into rare gas element, obtain the nitrating Graphene.
Pore-forming material is a kind of or its arbitrary combination in volatile salt, bicarbonate of ammonia, ammonium nitrate, ammonium sulfate, monoammonium sulfate, ammonium sulphite, ammonium chloride.
In the supersound process process, graphite oxide is by the ultrasonic graphene oxide that is dispersed into, and simultaneously, inorganic nitrogenous substances obtains mixing uniformly fully with graphene oxide.
The temperature of drying treatment is 40～60 ℃, and be 24～48h time of drying.
In the reduction reaction process, under the effect of high temperature, the functional group on graphene oxide surface decomposes generation CO
2deng gas, gas produces abundant hole after overflowing on graphene oxide, simultaneously, inorganic nitrogenous substances is decomposes effusion nitrogenous gas also, also produce pore space structure on inorganic nitrogenous substances, and the nitrogenous gas of overflowing enters doping in the defective graphene sheet layer of self tool, make the nitrating Graphene.
Reduction reaction is carried out in high temperature process furnances.
Rare gas element is argon gas, nitrogen or helium, or the mixed gas of any two kinds in argon gas, nitrogen and helium.
The preparation method of a kind of nitrating Graphene provided by the invention, enter nitrogen-doping in graphene sheet layer the nitrating Graphene that makes vesicular structure.These preparation method's raw material sources are wide, cost is low, simple to operation, and equipment, without particular requirement, is easy to mass and produces.Introduce nitrogen-atoms in the lamella of Graphene in the nitrating Graphene that this preparation method makes, nitrogen-atoms and C atomic linkage, can effectively realize that Graphene is from the semi-metal of zero band gap to semi-conductive transformation, and this nitrating Graphene has abundant hole, this vesicular structure has increased the specific surface area of nitrating Graphene and has had good mass transfer effect, therefore good conductivity, have good ion electronic conductivity, can be applicable to lithium ion-gas battery electrode and cathode of lithium battery etc.
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment mono-
A kind of preparation method of nitrating Graphene comprises the following steps:
The standby graphite oxide of the graphite-made that to get purity be 99.5%, its concrete steps are:
20g 50 order graphite, 10g Potassium Persulphate and 10g Vanadium Pentoxide in FLAKES are added in the vitriol oil of 80 ℃, stir, cooling 6h, washing is to neutral, drying; Dried sample is added in 0 ℃, the vitriol oil of 230mL, then add 60g potassium permanganate, the temperature of mixture to remain on 20 ℃, after then in the oil bath of 35 ℃, keeping 2h, slowly add the 920mL deionized water; After 15min, add again 2.8L deionized water (wherein containing the hydrogen peroxide that 50mL concentration is 30%), the mixture color becomes glassy yellow afterwards, and suction filtration, then the hydrochloric acid that is 10% by 5L concentration is while hot washed, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.
The beaker that the amount of trying to please is 1L, add the volatile salt of 1g graphite oxide and 0.1g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 1g/L, be put in ultrasonic apparatus ultrasonic 30 minutes by beaker, obtain volatile salt and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 60 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under nitrogen protection and reduced, describedly be reduced at 500 ℃ of temperature reduction 30 minutes, stop subsequently heating; naturally cool to room temperature, stop passing into nitrogen, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
The SEM Electronic Speculum figure that Fig. 1 is the prepared nitrating Graphene of the embodiment of the present invention one, as can be seen from Figure 1, Graphene thickness is about 1～3nm, and there is abundant hole on surface, and bore hole size is about 50nm not to be waited to the hundreds of nanometer.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 27*10
5s/m
Embodiment bis-
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the ammonium nitrate of 1g graphite oxide and 0.2g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 0.1g/L, be put in ultrasonic apparatus ultrasonic 60 minutes by beaker, obtain ammonium nitrate and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 40 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under argon shield and reduced, describedly be reduced at 680 ℃ of temperature reduction 1 minute, stop subsequently heating; naturally cool to room temperature, stop passing into argon gas, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 1.2*10
5s/m.
Embodiment tri-
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the bicarbonate of ammonia of 1g graphite oxide and 0.01g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 10g/L, be put in ultrasonic apparatus ultrasonic 50 minutes by beaker, obtain bicarbonate of ammonia and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 50 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under helium protection and reduced, describedly be reduced at 550 ℃ of temperature reductase 12 0 minute, stop subsequently heating; naturally cool to room temperature, stop passing into helium, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 4.3*10
5s/m.
Embodiment tetra-
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the ammonium sulfate of 1g graphite oxide and 0.05g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 2g/L, be put in ultrasonic apparatus ultrasonic 40 minutes by beaker, obtain ammonium sulfate and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 55 ℃, quartz boat is moved on in Reaktionsofen;
Getting dried described filter residue is placed under the volume ratio nitrogen/argon gas of 1: 1 protection and is reduced; described being reduced at 600 ℃ of temperature reduced 10 minutes; stop subsequently heating; naturally cool to room temperature; stop passing into the volume ratio nitrogen/argon gas of 1: 1; open Reaktionsofen, collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 0.8*10
5s/m.
Embodiment five
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the ammonium chloride of 1g graphite oxide and 0.5g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 0.5g/L, be put in ultrasonic apparatus ultrasonic 30 minutes by beaker, obtain ammonium chloride and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 45 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under nitrogen protection and reduced, describedly be reduced at 650 ℃ of temperature reduction 3 minutes, stop subsequently heating; naturally cool to room temperature, stop passing into nitrogen, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 3.1*10
5s/m.
Embodiment six
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the monoammonium sulfate of 1g graphite oxide and 0.3g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 5g/L, be put in ultrasonic apparatus ultrasonic 35 minutes by beaker, obtain monoammonium sulfate and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 48 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under nitrogen protection and reduced, describedly be reduced at 620 ℃ of temperature reduction 5 minutes, stop subsequently heating; naturally cool to room temperature, stop passing into nitrogen, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 1.9*10
5s/m.
Embodiment seven
A kind of preparation method of nitrating Graphene comprises the following steps:
The beaker that the amount of trying to please is 1L, add the ammonium sulphite of 1g graphite oxide and 0.1g in beaker, the solution that to add deionized water to be made into by graphite oxide concentration be 8g/L, be put in ultrasonic apparatus ultrasonic 45 minutes by beaker, obtain ammonium sulphite and graphene oxide mixing solutions, after filtering, collect filter residue;
Take out and be placed on quartz boat after described filter residue is dry under 50 ℃, quartz boat is moved on in Reaktionsofen;
Get dried described filter residue and be placed under nitrogen protection and reduced, describedly be reduced at 580 ℃ of temperature reduction 15 minutes, stop subsequently heating; naturally cool to room temperature, stop passing into nitrogen, open Reaktionsofen; collect solid product, described solid product is the nitrating Graphene.
Through the test of four point probe resistance meter, the specific conductivity of the nitrating Graphene that the present embodiment makes is 2.3*10
5s/m.
Claims (4)
1. the preparation method of a nitrating Graphene, is characterized in that, comprises the following steps:
The ratio that to get pore-forming material be 0.01～0.5: 1 with graphite oxide in mass ratio is soluble in water after mixing, and supersound process 30～60 minutes, make the mixing solutions that concentration is 0.1～10g/L; Then filter, collect screening and screening is carried out to drying treatment, make powder;
Under protection of inert gas, described dried powder is placed at 500～580 ℃ of temperature to reduce and processes 1～30 minute, stop subsequently heating, naturally cool to room temperature, stop passing into rare gas element, obtain the nitrating Graphene.
2. the preparation method of nitrating Graphene as claimed in claim 1, is characterized in that, described pore-forming material is a kind of or its arbitrary combination in volatile salt, bicarbonate of ammonia, ammonium nitrate, ammonium sulfate, monoammonium sulfate, ammonium sulphite, ammonium chloride.
3. the preparation method of nitrating Graphene as claimed in claim 1, is characterized in that, the temperature of described drying treatment is 40～60 ℃, and be 24～48h time of drying.
4. the preparation method of nitrating Graphene as claimed in claim 1, is characterized in that, described rare gas element is argon gas, nitrogen or helium, or the mixed gas of any two kinds in argon gas, nitrogen and helium.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104129781A (en) * | 2014-07-25 | 2014-11-05 | 深圳新宙邦科技股份有限公司 | In-situ nitrogen-doped porous graphene and preparation method thereof |
| CN104495825A (en) * | 2014-12-17 | 2015-04-08 | 北京科技大学 | Method for preparing porous nanometer graphite |
| CN104787751A (en) * | 2014-01-16 | 2015-07-22 | 中国科学院宁波材料技术与工程研究所 | Graphene powder and preparation method thereof |
| CN104891483A (en) * | 2015-06-03 | 2015-09-09 | 常州大学 | Preparation method of three-dimensional graphene |
| CN105800599A (en) * | 2016-02-29 | 2016-07-27 | 武汉理工大学 | Method for preparing nitrogen-auto-doped porous graphene by utilizing porous soybean hulls |
| CN106315563A (en) * | 2016-07-27 | 2017-01-11 | 中国科学院宁波材料技术与工程研究所 | Graphene material of ordered structure and preparing method thereof |
| CN106744827A (en) * | 2016-11-22 | 2017-05-31 | 华中科技大学 | A kind of method for carrying out controllable pore-creating to Graphene using microwave burning |
| CN107161964A (en) * | 2017-06-26 | 2017-09-15 | 北京石油化工学院 | A kind of method for preparing N doping phosphorus alkene |
| CN107416801A (en) * | 2017-09-08 | 2017-12-01 | 安徽玄同工业设计有限公司 | A kind of preparation method of the poroid graphene of three-dimensional |
| CN109336098A (en) * | 2018-09-30 | 2019-02-15 | 西安工业大学 | Porous N doped graphene of multilayer self-supporting and preparation method thereof |
| CN109755599A (en) * | 2018-12-14 | 2019-05-14 | 上海理工大学 | A kind of preparation method of graphene oxide-loaded Fe-N-C material |
| CN109768261A (en) * | 2019-01-25 | 2019-05-17 | 东北大学 | A kind of novel cathode material for lithium ion battery N doping porous graphene preparation method and application |
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| CN102120572A (en) * | 2011-01-24 | 2011-07-13 | 南京大学 | Method for preparing nitrogen-doped graphene |
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| CN104787751B (en) * | 2014-01-16 | 2017-11-03 | 中国科学院宁波材料技术与工程研究所 | A kind of graphene powder and preparation method thereof |
| CN104787751A (en) * | 2014-01-16 | 2015-07-22 | 中国科学院宁波材料技术与工程研究所 | Graphene powder and preparation method thereof |
| CN104129781B (en) * | 2014-07-25 | 2016-04-13 | 深圳新宙邦科技股份有限公司 | A kind of situ Nitrogen Doping porous graphene and preparation method thereof |
| CN104129781A (en) * | 2014-07-25 | 2014-11-05 | 深圳新宙邦科技股份有限公司 | In-situ nitrogen-doped porous graphene and preparation method thereof |
| CN104495825A (en) * | 2014-12-17 | 2015-04-08 | 北京科技大学 | Method for preparing porous nanometer graphite |
| CN104495825B (en) * | 2014-12-17 | 2016-08-24 | 北京科技大学 | A kind of preparation method of porous nano graphite |
| CN104891483A (en) * | 2015-06-03 | 2015-09-09 | 常州大学 | Preparation method of three-dimensional graphene |
| CN105800599A (en) * | 2016-02-29 | 2016-07-27 | 武汉理工大学 | Method for preparing nitrogen-auto-doped porous graphene by utilizing porous soybean hulls |
| CN106315563A (en) * | 2016-07-27 | 2017-01-11 | 中国科学院宁波材料技术与工程研究所 | Graphene material of ordered structure and preparing method thereof |
| CN106744827A (en) * | 2016-11-22 | 2017-05-31 | 华中科技大学 | A kind of method for carrying out controllable pore-creating to Graphene using microwave burning |
| CN106744827B (en) * | 2016-11-22 | 2018-12-28 | 华中科技大学 | A method of controllable pore-creating being carried out to graphene using microwave burning |
| CN107161964A (en) * | 2017-06-26 | 2017-09-15 | 北京石油化工学院 | A kind of method for preparing N doping phosphorus alkene |
| CN107416801A (en) * | 2017-09-08 | 2017-12-01 | 安徽玄同工业设计有限公司 | A kind of preparation method of the poroid graphene of three-dimensional |
| CN109336098A (en) * | 2018-09-30 | 2019-02-15 | 西安工业大学 | Porous N doped graphene of multilayer self-supporting and preparation method thereof |
| CN109755599A (en) * | 2018-12-14 | 2019-05-14 | 上海理工大学 | A kind of preparation method of graphene oxide-loaded Fe-N-C material |
| CN109768261A (en) * | 2019-01-25 | 2019-05-17 | 东北大学 | A kind of novel cathode material for lithium ion battery N doping porous graphene preparation method and application |
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Application publication date: 20131218 |