CN103145122A - Preparation method of nitrogen-doped graphene - Google Patents
Preparation method of nitrogen-doped graphene Download PDFInfo
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- CN103145122A CN103145122A CN2013100980289A CN201310098028A CN103145122A CN 103145122 A CN103145122 A CN 103145122A CN 2013100980289 A CN2013100980289 A CN 2013100980289A CN 201310098028 A CN201310098028 A CN 201310098028A CN 103145122 A CN103145122 A CN 103145122A
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Abstract
The invention relates to a preparation method of nitrogen-doped graphene, belonging to field of material synthesis. The preparation method performs hydrothermal treatment on a mixed solution of hydrazine hydrate and graphene oxide and prepares the nitrogen-doped graphene by taking the hydrazine hydrate as a reducing agent and a nitrogen source. By controlling the reaction conditions such as mass ratio of raw materials, reaction temperature and reaction time, the nitrogen-doped graphene with different nitrogen contents can be prepared. The nitrogen content of the nitrogen-doped graphene prepared by the method is 3.9-5.7wt%, and the carbon-oxygen ratio is 12-16%. The preparation method provided by the invention has simple flow, low energy consumption and high yield, and is easy to control and reproduce and is remarkably easy to popularize and use.
Description
Technical field
The invention belongs to material synthetic chemistry field, relate to a kind of preparation method of nitrogen-doped graphene, be specifically related to a kind of method for preparing nitrogen-doped graphene with hydro-thermal reaction.
Background technology
nitrogen-doped graphene is a kind of Graphene of elemental nitrogen modification, has the N-shaped characteristic of semiconductor, good reactive behavior and electrocatalysis characteristic, at transistor, fuel cell, lithium ion battery, biosensor, the fields such as ultracapacitor have important using value (Haibo Wang, Thandavarayan Maiyalagan, and Xin Wang, Review on recent progress in nitrogen-doped graphene:synthesis, characterization, and its potential applications[J], ACS Catalysis, 2 (2012) 781-794.).The preparation of nitrogen-doped graphene and performance study have perspective and applicability, have good prospect.
Document " Donghui Long; Wei Li; Licheng Ling; Jin Miyawaki; Isao Mochida; and Seong-Ho Yoon, Preparation of Nitrogen-Doped Graphene Sheets by a Combined Chemical and Hydrothermal Reduction of Graphene Oxide[J], Langmuir26 (2010): 16096-16102 " by the mixing solutions of hydrothermal treatment consists graphene oxide, hydrazine hydrate and ammoniacal liquor, prepare nitrogen-doped graphene.The method has the reaction raw materials complexity, the shortcoming of reaction conditions strict (pH=10).
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of preparation method of nitrogen-doped graphene, and this preparation method has that reaction raw materials is simple, and reaction conditions is simple, and productive rate is high, and energy consumption is low, and is easy to control, the advantage of easily reappearing.
Technical scheme
A kind of preparation method of nitrogen-doped graphene is characterized in that step is as follows:
The aqueous dispersions of step 1, preparation graphene oxide:
Mix the crystalline graphite powder of 3g and the NaNO of 1.5g in every part of vitriol oil
3, cooling 3h in ice-water bath then makes system temperature be upgraded to 0 ℃; Keep system temperature below 20 ℃, add the KMnO of 9g in the mixing solutions
4Then move into oil bath pan, after keeping 2h under 35 ℃ of constant temperature, add deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Use respectively 10% hydrochloric acid and distilled water repetitive scrubbing, suction filtration, dialysis gained sticky solid approaches neutral to the pH value; Dry, grinding gained solid get graphite oxide;
Take 60～140mg graphite oxide and insert in 60～70mL distilled water, with ultrasonic cleaner ultra-sonic dispersion 2h, being mixed with concentration is the aqueous dispersions of the deep yellow graphene oxide of 1～2mg/mL;
The mixing solutions of step 2, preparation graphene oxide and hydrazine hydrate: measure 1～2mL hydrazine hydrate solution, pour in the aqueous dispersions of the graphene oxide that step 1 prepares, magnetic force heated and stirred 10min, obtain uniform mixing solutions, wherein the volume ratio of graphene oxide aqueous dispersions and hydrazine hydrate solution is 30～70 ︰ 1;
The mixing solutions of step 3, hydrothermal treatment consists graphene oxide and hydrazine hydrate: step 2 gained mixing solutions is moved in stainless steel hydro-thermal still, and controlling compactedness is 70～80%; The sealing water heating kettle is placed in baking oven, and it is 160～200 ℃ that hydrothermal temperature is set, and the hydro-thermal reaction time is 8～12h; Reaction naturally cools to room temperature after finishing;
Step 4: open water heating kettle, take out reaction product, filter, repeatedly clean three times with distilled water, ethanol, acetone respectively, at 60 ℃ of vacuum-drying 24h, collect the black powder, get nitrogen-doped graphene.
Power during described ultrasonic cleaner ultra-sonic dispersion is 300W, and frequency is 40KHz.
Described hydrazine hydrate solution is 80wt.%.
Beneficial effect
The preparation method of a kind of nitrogen-doped graphene that the present invention proposes, beneficial effect is:
(1) in the preparation method who adopts, raw material is simple: only adopting hydrazine hydrate is raw material, both as nitrogenous source, again as reductive agent, adopts hydro-thermal reaction to realize original position hydrogen reduction and the nitrogen doping of graphene oxide.
(2) in the preparation method who adopts, reaction conditions is simple: without particular requirement, the preparation method is simple and easy to do to the pH value of reaction soln.
(3) the hydro-thermal technical process of adopting is simple, only needs a water heating kettle, and low for equipment requirements, with low cost, reaction process is easy to control, and influence factor is less, and favorable reproducibility is produced on a large scale, and its technology of preparing is very easily promoted the use of.
(4) hydrothermal temperature that adopts is lower, and energy consumption is low, save energy.
(5) the present invention can be according to the needs to product property, the conditions such as feed change mass ratio, temperature of reaction, time, preparation different nitrogen contents (3.9～5.7wt.%) nitrogen-doped graphene; Carbon-to-oxygen ratio can reach 12～16% simultaneously.
(6) productive rate of nitrogen-doped graphene is generally at 90%-95%.
Description of drawings
Fig. 1: the stereoscan photograph that is the prepared nitrogen-doped graphene of the embodiment of the present invention 3;
Fig. 2: be the transmission electron microscope photo of the prepared nitrogen-doped graphene of the embodiment of the present invention 3;
Fig. 3: for the x-ray photoelectron of graphene oxide and the prepared nitrogen-doped graphene of the embodiment of the present invention 3 can spectrogram.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1
(1) preparation of the aqueous dispersions of graphene oxide: flask is positioned in ice-water bath, pours the appropriate vitriol oil into; With 3g crystalline graphite powder, 1.5g NaNO
3Pour in flask, stir, cooling 3h then, making system temperature is 0 ℃; Add 9g KMnO in mixing solutions
4, stir, during keep system temperature below 20 ℃; Flask is moved into oil bath pan, after 35 ℃ of constant temperature 2h, add deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use respectively 10% hydrochloric acid and distilled water repetitive scrubbing, suction filtration, dialysis gained sticky solid approaches neutral to the pH value; Dry, grinding gained solid namely get graphite oxide; Take the 60mg graphite oxide, measure 60mL distilled water, pour in beaker, disperse 2h with conventional ultrasound cleanser ultrasonic (40KHz, 300W), being mixed with concentration is the aqueous dispersions of the deep yellow graphene oxide of 1mg/mL.
(2) mixing solutions of preparation graphene oxide and hydrazine hydrate: measure 1mL hydrazine hydrate solution (80wt.%), pour in the aqueous dispersions of the graphene oxide that step 1 prepares, magnetic force heated and stirred 10min, obtain uniform mixing solutions, wherein the volume ratio of graphene oxide aqueous dispersions and hydrazine hydrate solution is 60:1;
(3) mixing solutions of hydrothermal treatment consists graphene oxide and hydrazine hydrate: step 2 gained mixing solutions is moved in stainless steel hydro-thermal still, and controlling compactedness is 75%; After the sealing water heating kettle, be positioned in baking oven; It is 180 ℃ that hydrothermal temperature is set, and the hydro-thermal reaction time is 10h; Reaction naturally cools to room temperature after finishing;
(4) processing of reaction product: open water heating kettle, take out reaction product, filter, repeatedly clean three times with distilled water, ethanol, acetone respectively, 60 ℃ of vacuum-drying 24h collect the black powder, namely get nitrogen-doped graphene.
The nitrogen content of the nitrogen-doped graphene that the present embodiment is prepared is 3.9wt.%, and carbon-to-oxygen ratio is 14.6%.
Embodiment 2
(1) preparation of the aqueous dispersions of graphene oxide: flask is positioned in ice-water bath, pours the appropriate vitriol oil into; With 3g crystalline graphite powder, 1.5g NaNO
3Pour in flask, stir, cooling 3h then, making system temperature is 0 ℃; Add 9g KMnO in mixing solutions
4, stir, during keep system temperature below 20 ℃; Flask is moved into oil bath pan, after 35 ℃ of constant temperature 2h, add deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use respectively 10% hydrochloric acid and distilled water repetitive scrubbing, suction filtration, dialysis gained sticky solid approaches neutral to the pH value; Dry, grinding gained solid namely get graphite oxide; Take the 70mg graphite oxide, measure 70mL distilled water, pour in beaker, disperse 2h with conventional ultrasound cleanser ultrasonic (40KHz, 300W), being mixed with concentration is the aqueous dispersions of the deep yellow graphene oxide of 1mg/mL.
(2) mixing solutions of preparation graphene oxide and hydrazine hydrate: measure 2mL hydrazine hydrate solution (80wt.%), pour in the aqueous dispersions of the graphene oxide that step 1 prepares, magnetic force heated and stirred 10min, obtain uniform mixing solutions, wherein the volume ratio of graphene oxide aqueous dispersions and hydrazine hydrate solution is 35:1;
(3) mixing solutions of hydrothermal treatment consists graphene oxide and hydrazine hydrate: step 2 gained mixing solutions is moved in stainless steel hydro-thermal still, and controlling compactedness is 80%; After the sealing water heating kettle, be positioned in baking oven; It is 160 ℃ that hydrothermal temperature is set, and the hydro-thermal reaction time is 8h; Reaction naturally cools to room temperature after finishing;
(4) processing of reaction product: open water heating kettle, take out reaction product, filter, repeatedly clean three times with distilled water, ethanol, acetone respectively, 60 ℃ of vacuum-drying 24h collect the black powder, namely get nitrogen-doped graphene.
The nitrogen content of the nitrogen-doped graphene that the present embodiment is prepared is 4.5wt.%, and carbon-to-oxygen ratio is 12.5%.
Embodiment 3
(1) preparation of the aqueous dispersions of graphene oxide: flask is positioned in ice-water bath, pours the appropriate vitriol oil into; With 3g crystalline graphite powder, 1.5g NaNO
3Pour in flask, stir, cooling 3h then, making system temperature is 0 ℃; Add 9g KMnO in mixing solutions
4, stir, during keep system temperature below 20 ℃; Flask is moved into oil bath pan, after 35 ℃ of constant temperature 2h, add deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use respectively 10% hydrochloric acid and distilled water repetitive scrubbing, suction filtration, dialysis gained sticky solid approaches neutral to the pH value; Dry, grinding gained solid namely get graphite oxide; Take the 140mg graphite oxide, measure 70mL distilled water, pour in beaker, disperse 2h with conventional ultrasound cleanser ultrasonic (40KHz, 300W), being mixed with concentration is the aqueous dispersions of the deep yellow graphene oxide of 2mg/mL.
(2) mixing solutions of preparation graphene oxide and hydrazine hydrate: measure 2mL hydrazine hydrate solution (80wt.%), pour in the aqueous dispersions of the graphene oxide that step 1 prepares, magnetic force heated and stirred 10min, obtain uniform mixing solutions, wherein the volume ratio of graphene oxide aqueous dispersions and hydrazine hydrate solution is 35:1;
(3) mixing solutions of hydrothermal treatment consists graphene oxide and hydrazine hydrate: step 2 gained mixing solutions is moved in stainless steel hydro-thermal still, and controlling compactedness is 80%; After the sealing water heating kettle, be positioned in baking oven; It is 200 ℃ that hydrothermal temperature is set, and the hydro-thermal reaction time is 12h; Reaction naturally cools to room temperature after finishing;
(4) processing of reaction product: open water heating kettle, take out reaction product, filter, repeatedly clean three times with distilled water, ethanol, acetone respectively, 60 ℃ of vacuum-drying 24h collect the black powder, namely get nitrogen-doped graphene.
The nitrogen content of the nitrogen-doped graphene that the present embodiment is prepared is 5.7wt.%, and carbon-to-oxygen ratio is 16.3%.
The electron scanning micrograph of the sample that present embodiment is prepared as shown in Figure 1, transmission electron microscope photo is as shown in Figure 2.As seen from the figure, product is laminate structure, has obvious stacking, curling and fold.The XPS spectrum figure of the XPS spectrum figure of the sample that present embodiment is prepared and graphene oxide raw material as shown in Figure 3.As can be seen from the figure, occur the N1s peak in prepared sample, confirmed the successful preparation of nitrogen-doped graphene; Simultaneously, than graphene oxide, the oxygen level of prepared nitrogen-doped graphene obviously reduces, and carbon-to-oxygen ratio obviously strengthens.
Claims (3)
1. the preparation method of a nitrogen-doped graphene is characterized in that step is as follows:
The aqueous dispersions of step 1, preparation graphene oxide:
Mix the crystalline graphite powder of 3g and the NaNO of 1.5g in every part of vitriol oil
3, cooling 3h in ice-water bath then makes system temperature be upgraded to 0 ℃; Keep system temperature below 20 ℃, add the KMnO of 9g in the mixing solutions
4Then move into oil bath pan, after keeping 2h under 35 ℃ of constant temperature, add deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Use respectively 10% hydrochloric acid and distilled water repetitive scrubbing, suction filtration, dialysis gained sticky solid approaches neutral to the pH value; Dry, grinding gained solid get graphite oxide;
Take 60～140mg graphite oxide and insert in 60～70mL distilled water, with ultrasonic cleaner ultra-sonic dispersion 2h, being mixed with concentration is the aqueous dispersions of the deep yellow graphene oxide of 1～2mg/mL;
The mixing solutions of step 2, preparation graphene oxide and hydrazine hydrate: measure 1～2mL hydrazine hydrate solution, pour in the aqueous dispersions of the graphene oxide that step 1 prepares, magnetic force heated and stirred 10min, obtain uniform mixing solutions, wherein the volume ratio of graphene oxide aqueous dispersions and hydrazine hydrate solution is 30～70 ︰ 1;
The mixing solutions of step 3, hydrothermal treatment consists graphene oxide and hydrazine hydrate: step 2 gained mixing solutions is moved in stainless steel hydro-thermal still, and controlling compactedness is 70～80%; The sealing water heating kettle is placed in baking oven, and it is 160～200 ℃ that hydrothermal temperature is set, and the hydro-thermal reaction time is 8～12h; Reaction naturally cools to room temperature after finishing;
Step 4: open water heating kettle, take out reaction product, filter, repeatedly clean three times with distilled water, ethanol, acetone respectively, at 60 ℃ of vacuum-drying 24h, collect the black powder, get nitrogen-doped graphene.
2. the preparation method of nitrogen-doped graphene according to claim 1, it is characterized in that: the power during described ultrasonic cleaner ultra-sonic dispersion is 300W, frequency is 40KHz.
3. the preparation method of nitrogen-doped graphene according to claim 1, it is characterized in that: described hydrazine hydrate solution is 80wt.%.
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Cited By (14)
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| CN103435034A (en) * | 2013-08-14 | 2013-12-11 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene based non-metallic oxygen reduction catalyst |
| CN103449419A (en) * | 2013-08-19 | 2013-12-18 | 中国科学院上海硅酸盐研究所 | Preparation method of nitrogen-doped graphene with ultrahigh lithium storage capacity |
| CN103723717A (en) * | 2014-01-03 | 2014-04-16 | 中国科学院山西煤炭化学研究所 | Preparation method of nitrogen-doped graphene thin film |
| CN103990484A (en) * | 2014-05-26 | 2014-08-20 | 西北工业大学 | Preparation method of nitrogen doped and graphene loaded Cu-Cu2O nanocomposites |
| CN104671232A (en) * | 2013-11-29 | 2015-06-03 | 上海悦达墨特瑞新材料科技有限公司 | Preparation method of graphene and application of prepared graphene |
| CN105217613A (en) * | 2015-10-15 | 2016-01-06 | 田野 | A kind of preparation method of Graphene dopant material and application |
| CN105696014A (en) * | 2016-03-16 | 2016-06-22 | 西安交通大学 | Nitrogen doped graphene N-rGO and nano lamella cluster MoSe2 composite structure and preparation method |
| US20160315194A1 (en) * | 2015-04-24 | 2016-10-27 | Daegu Gyeongbuk Institute Of Science And Technology | Preparation method of reduced and n-doped graphene oxide and the reduced and n-doped graphene oxide thereby |
| CN107857253A (en) * | 2017-12-04 | 2018-03-30 | 内蒙古科技大学 | A kind of three-dimensional porous graphene of N doping and preparation method thereof |
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| CN109888316A (en) * | 2019-03-14 | 2019-06-14 | 内蒙古科技大学 | Nitrogen-doped graphene prepares the method for catalyst, the preparation method of working electrode and its working electrode |
| CN110071290A (en) * | 2019-05-17 | 2019-07-30 | 江苏海基新能源股份有限公司 | A kind of preparation method of graphene conductive slurry |
| CN110155998A (en) * | 2019-05-13 | 2019-08-23 | 东南大学 | A kind of ribbon nitrogen-doped graphene and its preparation method and application |
| CN110562970A (en) * | 2019-06-20 | 2019-12-13 | 昆明物理研究所 | Preparation method of bromine-doped graphene oxide |
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| CN103449419A (en) * | 2013-08-19 | 2013-12-18 | 中国科学院上海硅酸盐研究所 | Preparation method of nitrogen-doped graphene with ultrahigh lithium storage capacity |
| CN103449419B (en) * | 2013-08-19 | 2015-05-13 | 中国科学院上海硅酸盐研究所 | Preparation method of nitrogen-doped graphene with ultrahigh lithium storage capacity |
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| CN103723717A (en) * | 2014-01-03 | 2014-04-16 | 中国科学院山西煤炭化学研究所 | Preparation method of nitrogen-doped graphene thin film |
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| US20160315194A1 (en) * | 2015-04-24 | 2016-10-27 | Daegu Gyeongbuk Institute Of Science And Technology | Preparation method of reduced and n-doped graphene oxide and the reduced and n-doped graphene oxide thereby |
| US9893199B2 (en) * | 2015-04-24 | 2018-02-13 | Daegu Gyeongbuk Institute Of Science And Technology | Preparation method of reduced and N-doped graphene oxide and the reduced and N-doped graphene oxide thereby |
| CN105217613A (en) * | 2015-10-15 | 2016-01-06 | 田野 | A kind of preparation method of Graphene dopant material and application |
| CN105696014A (en) * | 2016-03-16 | 2016-06-22 | 西安交通大学 | Nitrogen doped graphene N-rGO and nano lamella cluster MoSe2 composite structure and preparation method |
| CN105696014B (en) * | 2016-03-16 | 2018-06-26 | 西安交通大学 | A kind of nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction and preparation method |
| CN107857253A (en) * | 2017-12-04 | 2018-03-30 | 内蒙古科技大学 | A kind of three-dimensional porous graphene of N doping and preparation method thereof |
| CN108101038A (en) * | 2017-12-23 | 2018-06-01 | 深圳大学 | A kind of preparation method of furazan analog derivative as the nitrogen-doped graphene of nitrogen source |
| CN108101038B (en) * | 2017-12-23 | 2021-06-01 | 深圳大学 | Preparation method of nitrogen-doped graphene with furazan derivatives as nitrogen source |
| CN109888316A (en) * | 2019-03-14 | 2019-06-14 | 内蒙古科技大学 | Nitrogen-doped graphene prepares the method for catalyst, the preparation method of working electrode and its working electrode |
| CN110155998A (en) * | 2019-05-13 | 2019-08-23 | 东南大学 | A kind of ribbon nitrogen-doped graphene and its preparation method and application |
| CN110155998B (en) * | 2019-05-13 | 2023-02-21 | 东南大学 | Strip-shaped nitrogen-doped graphene and preparation method and application thereof |
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| CN110562970A (en) * | 2019-06-20 | 2019-12-13 | 昆明物理研究所 | Preparation method of bromine-doped graphene oxide |
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Application publication date: 20130612 |