CN106946247A - A kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis - Google Patents
A kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis Download PDFInfo
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- CN106946247A CN106946247A CN201710108192.1A CN201710108192A CN106946247A CN 106946247 A CN106946247 A CN 106946247A CN 201710108192 A CN201710108192 A CN 201710108192A CN 106946247 A CN106946247 A CN 106946247A
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Abstract
The invention discloses a kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis, obtain exposing the graphene oxide raw material of more edge active positions using nanosecond laser irradiating soln, raw material can be regulated and controled by laser energy and exposure time with exposed edge active position, more controllable pyridine N structures can be obtained in later stage Hydrothermal Synthesiss nitrogen-doped graphene, to lift the catalytic activity of nitrogen-doped graphene.The present invention takes the lead in the method for proposing pyridine nitrogen content in a kind of controllable lifting nitrogen-doped graphene, the method that the synthesis of nitrogen of high activity doped graphene is realized in the aqueous phase under benign environment.In addition, synthetic method craft of the present invention be simple and convenient to operate, it is easily controllable, and be not used poisonous reaction raw materials, be a kind of environment-friendly green synthesis process.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen-doped graphene, more particularly to a kind of laser irradiation synthesis is more active
The preparation method of position nitrogen-doped graphene.
Background technology
Currently, the energy crisis and environmental problem that fossil fuel is brought are increasingly serious, and more and more concern can by people
The exploitation of the renewable sources of energy.The key technology that regenerative resource changes with storing includes fuel cell, chargeable metal-air
Battery, photocatalytic water etc., and its key problem is to find efficient, cheap oxygen reduction reaction (ORR) and oxygen evolution reaction (OER)
Catalyst, to replace expensive and rare storage noble metal (Pt, Pt alloy) and its oxide (IrO2、RuO2), this for
Promoting the commercialization process of renewable energy utilization technology has and its important meaning.The carbon material enriched based on the earth, one
Kind of the carbon-based non-metal catalyst of new catalyst be found to be it is a kind of efficiently, low cost, no metal and alternative platinum is used to fire
Expect the catalyst of the oxygen reduction reaction in battery, wherein nitrogen-doped graphene has proven to carbon-based without very effective in metal
The catalyst of oxygen reduction reaction.
Since 2009, nitrogen-doped carbon nanometer pipe was reported with efficient oxygen reduction catalytic activity while also having for the first time
There are the methanol tolerance and stability better than platinum carbon, the oxygen reduction catalytic activity of carbon-based non-metal catalyst is obtained extensively from there on
General research.Then N doping, sulfur doping, phosphorus doping, I2 doping graphene and edge halogenation doped graphite are reported in succession
The high-efficiency catalytic activity that alkene has in oxygen reduction reaction.Wherein, Dai et al. first reported nitrogen-doped carbon nanometer pipe have it is good
Good catalytic activity and the stability and methanol tolerance better than platinum carbon.Referring to：Kuanping Gong,Feng Du,
Liming Dai.Science 323,760–764(2009).Subsequent Yang et al. and Jeon etc. reports sulfur doping, phosphorus in succession
Doping, the performance of I2 doping graphene and edge halogenation doped graphene in oxygen reduction reaction.
At present, nitrogen-doped graphene is main study hotspot.Dai et al. passed through CVD synthetic nitrogen first in 2010
Doped graphene, shows good oxygen reduction catalytic activity.Referring to：Kuanping Gong,Feng Du,Liming
Dai.ACS Nano 4,1321–1326(2010)；James in 2014 et al. on graphene oxide by growing graphite oxide
The nitrogen-doped graphene of the more marginal textures of alkene quantum dot synthesis tool, tests the catalysis that obtained result is nitrogen-doped graphene and lives
Property, which has, to be obviously improved, referring to：Huilong Fei,James M.Tour.ACS Nano 10,10837–10843(2014)；
Zhang et al. carries out theoretical modeling, gained knot using density functional theory to the mechanism of oxygen reduction reaction on nitrogen-doped graphene
Fruit is consistent with Germicidal efficacy, i.e., ORR is direct 4 electronic channel on NG；Guo in 2016 et al., which passes through, tests card pyridine
Nitrogen is the key for lifting oxygen reduction reaction catalytic activity.Referring to：Guo,D.H.et al.Science 351,361–365
(2016).But up to the present, synthesize nitrogen-doped graphene condition it is harsher, and not someone's system research how
The pyridine nitrogen content of nitrogen-doped graphene is lifted to lift the catalytic activity of material.
The content of the invention
In order to solve problems of the prior art, the present invention provides a kind of laser irradiation synthesis many active sites N dopings
The preparation method of graphene, overcome in the prior art synthesis technique can not be synthesized under low-temp low-pressure there is high-efficiency catalytic activity
Nitrogen-doped graphene and the problem of can not effectively control pyridine nitrogen content in nitrogen-doped graphene.
The technical solution adopted by the present invention is：
A kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis, comprises the following steps：
(1) graphene oxide prepared using improved Hummers methods as raw material, by graphene oxide and ethanol solution with
1mg:1ml~1mg：10ml ratios are mixed, and ultrasonication is uniform；
(2) 10~50ml of sample obtained by step (1) is put into conical flask, with nanosecond parallel pulse laser irradiation 10~
50min solution；
(3) sample obtained by step (2) is subjected to high speed centrifugation, 12000~20000 revs/min of rotating speed obtains precipitating simultaneously
It is lyophilized；
(4) by the sample and ammonium hydrogen carbonate obtained by step (3) with mass ratio 1:1~1:50 mixing are soluble in water, will be mixed
Close solution to pour into reactor, reacted 5~20 hours at a temperature of 90~200 DEG C；
(5) by the sample centrifugation obtained by step (4), washing three times, freeze.
During step (2) the ps pulsed laser and ns pulsed laser effect irradiation, the energy of laser is 270mJ, and wavelength is 1064nm, laser
Repetition rate is 10Hz.
To be stirred in step (2) the laser irradiation process, mixing speed is controlled at 500 revs/min -800 revs/min,
So that solution is dispersed.
Whole preparation process is carried out all in exposed environment, without being passed through protection gas.
The beneficial effects of the invention are as follows：The present invention obtains exposing more edge active positions using nanosecond laser irradiating soln
Graphene oxide raw material, can regulate and control raw material with exposed edge active position, in later stage water by laser energy and exposure time
More controllable pyridine N structures can be obtained during thermal synthesis nitrogen-doped graphene, to lift the catalysis work of nitrogen-doped graphene
Property.The present invention takes the lead in the method for proposing pyridine nitrogen content in a kind of controllable lifting nitrogen-doped graphene, under benign environment
The method that the synthesis of nitrogen of high activity doped graphene is realized in aqueous phase.In addition, synthetic method craft letter of the present invention
It is single, easy to operate, easily controllable, and poisonous reaction raw materials are not used, it is a kind of environment-friendly green synthesis process.
Brief description of the drawings
Fig. 1 is the process device figure that more edge active positions are exposed using nanosecond laser irradiation oxidation graphene；
Fig. 2 (a) is the low power transmission electron microscope photo of raw material graphene oxide；(b) it is the irradiated rear oxidation of laser
Graphene low power transmission electron microscope photo；(c) the irradiated rear oxidation graphene high power transmission electron microscope photo of laser；
(d) scheme for the Raman of laser predose rear oxidation graphene；
Fig. 3 (a) is the nitrogen-doped graphene irradiated without laser, the nitrogen-doped graphene synthesized after (b) laser treatment
X-ray photoelectron spectroscopic analysis figure；Analyze data find laser irradiation after pyridine nitrogen content by before 24% lifting to
53%, improve 120%；
Fig. 4 be the oxygen of nitrogen-doped graphene synthesized after the nitrogen-doped graphene and laser treatment irradiated without laser also
Originality energy comparison diagram, wherein (a) is the polarization curve of oxygen reduction reaction, (b) is the tafel slopes of oxygen reduction reaction, and (c) is
Dynamics current density and electron transfer number, (d) is that methanol tolerance should；It can be seen that the nitrogen-doped graphene after laser irradiation
Take-off potential improves 60mv, and diffusion current density is by 4.6mA/cm before2Lift 5.3mA/cm2, electron transfer number is by it
3.78 preceding liftings are to 3.95, and dynamics current density is by 8.2mA/cm before2Lift 17.6mA/cm2, tafel slopes
From 72mv/dec liftings to 56mv/dec, and still keep good methanol tolerance.
Embodiment
As shown in Fig. 1 synthesizer figures, the mixing speed of magneton should not be too slow also unsuitable too fast, and too time slack solution is mixed not
Uniformly, it may sputter out soon very much solution, mixing speed is suitable to control between 500 revs/min -800 revs/min.Receive
When pulse per second (PPS) laser action is irradiated, the energy of laser is 270mJ, and wavelength is 1064nm, and laser repetition rate is 10Hz.Whole system
Standby process is carried out all in exposed environment, without being passed through protection gas.
Embodiment 1：
The preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis, comprises the following steps：
(1) graphene oxide 10mg is dissolved in 20ml by the graphene oxide using the preparation of improved Hummers methods as raw material
Ethanol solution in (analysis pure), crush five minutes under conditions of 400w power is broken, then ultrasonic vibration 10 minutes.
(2) 20ml is taken to be put into conical flask in the sample obtained by step (1), with nanosecond parallel veins impulse actinometric solutions,
Time is 10min.
(3) sample obtained by step (2) is subjected to (16000 revs/min) centrifugation 25min at a high speed, is precipitated and freezed.
(4) the sample 10mg obtained by step (3) is dissolved in 30ml water and adds 100mg ammonium hydrogen carbonate, by mixed solution
Pour into 40ml reactors, reacted 12 hours at a temperature of 90 DEG C.
(5) by the sample centrifugation obtained by step (4), washing three times, centrifuge 20 minutes, freeze under 20000 revs/min of rotating speed
It is dry.
Embodiment 2：
The preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis, comprises the following steps：
(1) graphene oxide 60mg is dissolved in by the graphene oxide using the preparation of improved Hummers methods as raw material
In 180ml ethanol solution (analysis pure), 40 minutes are crushed under conditions of 300w power is broken, then 20 points of ultrasonic vibration
Clock.
(2) 30ml is taken to be put into conical flask in the sample obtained by step (1), with nanosecond parallel veins impulse actinometric solutions,
Time is 30min.
(3) sample obtained by step (2) is subjected to (20000 revs/min) centrifugation 30min at a high speed, is precipitated and freezed.
(4) the sample 15mg obtained by step (3) is dissolved in 30ml water and adds 75mg ammonium hydrogen carbonate, mixed solution is fallen
Enter in 40ml reactors, reacted 12 hours at a temperature of 150 DEG C.
(5) by the sample centrifugation obtained by step (4), washing three times, centrifuged 20 minutes under 20000 revs/min of rotating speed.
Embodiment 3：
The preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis, comprises the following steps：
(1) graphene oxide 30mg is dissolved in by the graphene oxide using the preparation of improved Hummers methods as raw material
In 300ml ethanol solution (analysis pure), 20 minutes are crushed under conditions of 450w power is broken, then 40 points of ultrasonic vibration
Clock.
(2) 40ml is taken to be put into conical flask in the sample obtained by step (1), with nanosecond parallel veins impulse actinometric solutions,
Time is 40min.
(3) sample obtained by step (2) is subjected to (18000 revs/min) centrifugation 35min at a high speed, is precipitated and freezed.
(4) the sample 20mg obtained by step (3) is dissolved in 80ml water and adds 1g ammonium hydrogen carbonate, mixed solution is poured into
In 100ml reactors, reacted 16 hours at a temperature of 200 DEG C.
(5) by the sample centrifugation obtained by step (4), washing three times, centrifuged 40 minutes under 20000 revs/min of rotating speed.
Although above in conjunction with figure, invention has been described, and the invention is not limited in above-mentioned specific embodiment party
Formula, above-mentioned embodiment is only schematical, rather than restricted, and one of ordinary skill in the art is in this hair
Under bright enlightenment, without deviating from the spirit of the invention, many variations can also be made, these belong to the guarantor of the present invention
Within shield.
Claims (4)
1. the preparation method of many active sites nitrogen-doped graphenes of a kind of laser irradiation synthesis, it is characterised in that comprise the following steps：
(1) graphene oxide using the preparation of improved Hummers methods is as raw material, by graphene oxide and ethanol solution with 1mg:
1ml~1mg：10ml ratios are mixed, and ultrasonication is uniform；
(2) 10~50ml of sample obtained by step (1) is put into conical flask, with nanosecond parallel pulse laser irradiation 10~
50min solution；
(3) sample obtained by step (2) is subjected to high speed centrifugation, 12000~20000 revs/min of rotating speed is precipitated and frozen
It is dry；
(4) by the sample and ammonium hydrogen carbonate obtained by step (3) with mass ratio 1:1~1:50 mixing are soluble in water, will mix molten
Liquid is poured into reactor, is reacted 5~20 hours at a temperature of 90~200 DEG C；
(5) by the sample centrifugation obtained by step (4), washing three times, freeze.
2. laser irradiation synthesizes the preparation method of many active sites nitrogen-doped graphenes according to claim 1, it is characterised in that
During step (2) the ps pulsed laser and ns pulsed laser effect irradiation, the energy of laser is 270mJ, and wavelength is 1064nm, laser repetition rate
For 10Hz.
3. laser irradiation synthesizes the preparation method of many active sites nitrogen-doped graphenes according to claim 1, it is characterised in that
To be stirred in step (2) the laser irradiation process, mixing speed is controlled at 500 revs/min -800 revs/min.
4. laser irradiation synthesizes the preparation method of many active sites nitrogen-doped graphenes according to claim 1, it is characterised in that
Whole preparation process is carried out all in exposed environment, without being passed through protection gas.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108914251A (en) * | 2018-07-09 | 2018-11-30 | 杭州高烯科技有限公司 | A kind of azepine graphite fibre and preparation method thereof |
| CN109279598A (en) * | 2018-11-16 | 2019-01-29 | 中科院合肥技术创新工程院 | A kind of method of liquid laser auxiliary synthesis heteroatom doped graphene aeroge |
| CN109289892A (en) * | 2018-09-30 | 2019-02-01 | 天津大学 | Manganese base mullite/nitrogen-doped graphene composite oxygen elctro-catalyst and preparation method |
| CN109590008A (en) * | 2018-12-25 | 2019-04-09 | 天津大学 | The preparation method of Laser synthesizing Lacking oxygen is adjustable cobaltosic oxide nitrogen-doped graphene |
| CN110040723A (en) * | 2019-04-26 | 2019-07-23 | 辽宁烯旺石墨科技有限公司 | A method of graphene is prepared using ion sputtering and laser complex technique |
| CN110586156A (en) * | 2019-09-03 | 2019-12-20 | 天津大学 | Preparation method for synthesizing mesoporous nitrogen-doped graphene-loaded molybdenum disulfide through laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electro-catalysis hydrogen production |
| CN110624587A (en) * | 2019-09-23 | 2019-12-31 | 天津大学 | Preparation method for synthesizing cobalt ferrite composite nitrogen-doped three-dimensional porous graphene with assistance of laser |
| CN113066976A (en) * | 2021-03-19 | 2021-07-02 | 中国科学院上海应用物理研究所 | Application of nitrogen-doped carbon nanotube in lithium ion battery cathode material |
| CN113725073A (en) * | 2020-05-25 | 2021-11-30 | 国家纳米科学中心 | Manufacturing method of nitrogen-doped graphene field effect transistor |
| CN113789663A (en) * | 2021-08-22 | 2021-12-14 | 北京工业大学 | Preparation method and application of N, F doped carbon material dual-function integrated catalyst |
| WO2023225921A1 (en) * | 2022-05-25 | 2023-11-30 | 北京小米移动软件有限公司 | Conductive agent processing method, conductive agent, electrode, and battery |
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| CN101844761A (en) * | 2010-05-28 | 2010-09-29 | 上海师范大学 | Method of adopting laser radiation for preparing reduction-oxidation graphene |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108914251A (en) * | 2018-07-09 | 2018-11-30 | 杭州高烯科技有限公司 | A kind of azepine graphite fibre and preparation method thereof |
| CN108914251B (en) * | 2018-07-09 | 2020-10-30 | 杭州高烯科技有限公司 | Nitrogen-doped graphite fiber and preparation method thereof |
| CN109289892A (en) * | 2018-09-30 | 2019-02-01 | 天津大学 | Manganese base mullite/nitrogen-doped graphene composite oxygen elctro-catalyst and preparation method |
| CN109289892B (en) * | 2018-09-30 | 2020-12-29 | 天津大学 | Manganese-based mullite/nitrogen-doped graphene composite oxygen electrocatalyst and preparation method thereof |
| CN109279598A (en) * | 2018-11-16 | 2019-01-29 | 中科院合肥技术创新工程院 | A kind of method of liquid laser auxiliary synthesis heteroatom doped graphene aeroge |
| CN109590008A (en) * | 2018-12-25 | 2019-04-09 | 天津大学 | The preparation method of Laser synthesizing Lacking oxygen is adjustable cobaltosic oxide nitrogen-doped graphene |
| CN110040723A (en) * | 2019-04-26 | 2019-07-23 | 辽宁烯旺石墨科技有限公司 | A method of graphene is prepared using ion sputtering and laser complex technique |
| CN110586156B (en) * | 2019-09-03 | 2022-06-10 | 天津大学 | Preparation method for synthesizing mesoporous nitrogen-doped graphene-loaded molybdenum disulfide through laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electro-catalysis hydrogen production |
| CN110586156A (en) * | 2019-09-03 | 2019-12-20 | 天津大学 | Preparation method for synthesizing mesoporous nitrogen-doped graphene-loaded molybdenum disulfide through laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electro-catalysis hydrogen production |
| CN110624587A (en) * | 2019-09-23 | 2019-12-31 | 天津大学 | Preparation method for synthesizing cobalt ferrite composite nitrogen-doped three-dimensional porous graphene with assistance of laser |
| CN113725073A (en) * | 2020-05-25 | 2021-11-30 | 国家纳米科学中心 | Manufacturing method of nitrogen-doped graphene field effect transistor |
| CN113066976A (en) * | 2021-03-19 | 2021-07-02 | 中国科学院上海应用物理研究所 | Application of nitrogen-doped carbon nanotube in lithium ion battery cathode material |
| CN113789663A (en) * | 2021-08-22 | 2021-12-14 | 北京工业大学 | Preparation method and application of N, F doped carbon material dual-function integrated catalyst |
| WO2023225921A1 (en) * | 2022-05-25 | 2023-11-30 | 北京小米移动软件有限公司 | Conductive agent processing method, conductive agent, electrode, and battery |
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