CN103526182A - Preparation method for nitrogen-doped graphene by utilization of nonmetal substrate surfaces - Google Patents
Preparation method for nitrogen-doped graphene by utilization of nonmetal substrate surfaces Download PDFInfo
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- CN103526182A CN103526182A CN201310518327.3A CN201310518327A CN103526182A CN 103526182 A CN103526182 A CN 103526182A CN 201310518327 A CN201310518327 A CN 201310518327A CN 103526182 A CN103526182 A CN 103526182A
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Abstract
Provided is a preparation method for nitrogen-doped graphene by utilization of nonmetal substrate surfaces. First, surfaces of a nonmetal substrate are cleaned, and then the nonmetal substrate is place in a high temperature section of a tubular type CVD system. Then the furnace temperature rises to 600-1000 DEG C in 15-30 min, and air is introduced during the above process. The nonmetal substrate is maintained in the above temperature range for 20-60 min. Then the furnace temperature is reduced slowly, and reaches the room temperature. The air in the furnace is then emptied. Then the furnace temperature rises to 1050-1500 DEG C in 40-120 min with hydrogen and high-purity argon as carrier gases. The nonmetal substrate is maintained at the temperature for 10-30 min. Then gases containing carbon and nitrogen sources are introduced for the growth of nitrogen-doped graphene. The nonmetal substrate is maintained at the temperature for 30-300 min. Finally, heating is stopped, the furnace temperature is reduced slowly to the room temperature. The method avoids introduction of impurities during following-up transfer processes.
Description
Technical field
A kind of method of preparing Graphene of the present invention, is specifically related to a kind of method of preparing nitrogen-doped graphene.
Background technology
Because si-substrate integrated circuit performance improves, be faced with further theoretical restriction, numerous researchists have directed one's energies to non-silica-base material to find can be applied to improve the unique material of electron device performance of future generation.Carbon nanomaterial has higher hope in replacement silicon technical field of electronic devices.
Unique physicals that recently Graphene has due to its perfect Two-dimensional Carbon atomic crystal structure and the extensive concern that has caused people as the potential using value of rear silicon-based nano field of electronic devices thereof.Graphene is the single carbon atom layer structure of graphite, and carbon atom skeleton is wherein arranged into hexagonal zero gap semiconductor structure.The carrier mobility (2 * 10 that Graphene is high
5cm
2v
-1s
-1) make it in high-frequency transistor field, there is important using value.On the other hand, utilize Graphene to lack band gap as the field-effect transistor of semiconductor channel, do not there is the function of regulation and control electric property, limited the application of its being on the scene effect field of transistors.Based on this, numerous study group change its electric property by mix heteroatomic method in Graphene internal structure, thereby obtain the graphene film material with semi-conductor electricity feature.Chemical doping normally utilizes heteroatoms to replace the carbon atom in Graphene internal structure, and move to negative pole or positive extreme direction the dirac point position that can effectively change Graphene by doping, thereby obtain N-shaped or p-type electricity structure field-effect transistor.
Because p-type graphene field effect transistor is easy to obtain, therefore how to prepare N-shaped field-effect transistor as transistorized the supplementing of p-type just seemed to very important in air or oxygen.
Current researchist has invented a large amount of methods and using nitrogen-atoms as Heteroatom doping, has entered the method for Graphene network.The lone-pair electron of nitrogen-atoms produce the high electron mobility with N-shaped electrical characteristic to Graphene and play important effect, by can effectively regulating and controlling its electrology characteristic to Graphene network contribution lone-pair electron.
The method of preparing at present nitrogen-doped graphene mainly contains chemical Vapor deposition process (CVD), solvent-thermal method, and electric heating doping method etc., wherein CVD method is used for preparing large-area high-quality nitrogen-doped graphene mould material in a large number.These utilize the standby nitrogen-doped graphene of CVD legal system is mainly to using transition metal substrate as catalyzer, as Copper Foil etc.Although utilize Copper Foil higher as the prepared nitrogen-doped graphene quality of catalyzer, and there is big area homogeneous characteristic, but because being is grown in metal substrate surface, therefore cannot be applied directly in electron device, need to be first obtained Graphene be transferred on specific substrate as polymethylmethacrylate (PMMA) etc. by intermediary.Owing to needing that before shifting copper catalyst used etc. is etched away in iron(ic) chloride or iron nitrate, this process can be introduced a large amount of impurity, in addition, utilizing acetone that medium PMMA is washed away in process, because PMMA can not remove totally completely, therefore impurity that also can be a large amount of at the remained on surface of nitrogen-doped graphene? how do we solve this problem of introducing of impurity in Graphene transfer process so? the best way is exactly in process of growth, not adopt the metal catalysts such as copper, but at nonmetal substrate surface direct growth nitrogen-doped graphene.
Therefore how to realize that at nonmetal substrate surface, directly to prepare nitrogen-doped graphene be this research field focus at present.This technology has advantages of environment protection, to reducing the application cost of nitrogen-doped graphene, realizes the application of nitrogen-doped graphene at aspects such as high-performance electronic devices and has huge pushing effect.
Summary of the invention
For overcoming deficiency of the prior art, object of the present invention aims to provide a kind of method of preparing nitrogen-doped graphene at nonmetal substrate surface.The method can be saved the transfer process of conventionally preparing after nitrogen-doped graphene, has avoided the introducing of impurity in subsequent transfer process, not only environmental protection but also can reduce it in the application cost of field of electronic devices.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
Nonmetal substrate surface is prepared a method for nitrogen-doped graphene, it is characterized in that, comprises the following steps:
Step 1) is cleaned the surface of the nonmetal substrate with certain surface terrain feature;
Step 2) at described nonmetal substrate surface, prepare nitrogen-doped graphene film, mainly comprise the following steps:
207) the described nonmetal substrate cleaning up is put into the high-temperature zone part of tubular type CVD system;
208) furnace temperature was elevated between 600-1000 ℃ in 15-30 minute, and passes into air in this process, and reach after setting between 600-1000 ℃ of temperature and maintain 20-60 minute in furnace temperature, slowly reduce subsequently furnace temperature, make it reach room temperature;
209) furnace air is got rid of totally;
210) take hydrogen and high-purity argon gas as carrier gas in the situation that, within the time of 40-120 minute, furnace temperature is elevated between 1050-1500 ℃, and described nonmetal substrate is kept to 10-30 minute at this temperature;
211) pass into the growth of carrying out nitrogen-doped graphene containing the gas of carbon and nitrogen sources, and maintain 30-300 minute at 1050-1500 ℃ of temperature;
212) stop heating, furnace temperature is slowly reduced to room temperature.
Further, the concrete grammar of step 1 is as follows: described nonmetal substrate is placed in to sulfuric acid/hydrogen peroxide (70/30) solution and carries out boiling for some time; Or, first utilize liquid detergent repeatedly to wash by rubbing with the hands the nonmetal substrate of institute, put into successively respectively subsequently the tap water that is dissolved with liquid detergent, tap water, intermediate water, then takes out and dries at supersound process for some time in ethanolic soln and acetone soln from acetone soln; Or above-mentioned two kinds of methods are also used.
Further, the concrete grammar of step 203 is as follows: with vacuum pump, the pressure in described tubular type CVD system is controlled to the low-pressure state below 10mTorr, then be filled with high-purity argon gas to normal pressure, with vacuum pump, its pressure is reduced to below 10mTorr more subsequently, several times so repeatedly, to process the air in pipe as far as possible totally; Or, directly in described tubular type CVD system, pass into the high-purity argon gas 30 minutes of 500sccm to as far as possible furnace air is got rid of clean; Or above-mentioned two kinds of methods are also used.
Preferably, furnace temperature is elevated between 1100-1300 ℃ in step 204.
Preferably, described in step 205, the gas containing carbon and nitrogen sources is methane and ammonia; The flow that passes into of described methane is 1-30sccm, and the flow that passes into of described ammonia is 10-50sccm.
Preferably, described nonmetal substrate is two dimensional structure, curved-surface structure or 3-D solid structure.
Preferably, described nonmetal substrate is concave surface or the artificial metamaterial structure of convex mirror structure, optical grating construction, optical waveguide structure, photon crystal structure or fishing net shaped.
Preferably, described nonmetal substrate is silicon base, silicon-dioxide substrate, the nitride silicon based end or sapphire substrates.
The invention has the beneficial effects as follows:
1, method of the present invention compared with prior art, without carrying out under reduced pressure, has reduced equipment cost, and prepared nitrogen-doped graphene film defect concentration is lower, has higher quality;
2, the size of the prepared nitrogen-doped graphene film of the present invention is only limited to the size of furnace inner space, nitrogen-doped graphene film that therefore can the required size of large-area preparation.
3, the present invention is owing to being directly to carry out the growth of nitrogen-doped graphene at nonmetal substrate surface, therefore the transfer process in the middle of having saved, avoided the use of chemical reagent to avoid the introducing of impurity in traditional transfer process simultaneously, this inventive method has reduced the preparation cost of respective electronic device in addition, make the more environmental protection of whole process, more energy-conservation, have more practicality.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, below with preferred embodiment of the present invention and coordinate accompanying drawing to be described in detail as follows.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms the application's a part, and schematic description and description of the present invention is used for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the CVD system and device schematic diagram of preparing nitrogen-doped graphene at nonmetal substrate surface for of the present invention.
Fig. 2 is that the present invention prepares the process of growth schematic diagram of nitrogen-doped graphene at nonmetal substrate surface.
Fig. 3 is the Raman spectrogram of the nitrogen-doped graphene prepared at nonmetal substrate surface of the present invention.
Number in the figure explanation: 1, nonmetal substrate, 2, tube furnace, 3, silica tube, 4, methane, 5, ammonia, 6, tail gas outlet.
Embodiment
Below with reference to the accompanying drawings and in conjunction with the embodiments, describe the present invention in detail.
Embodiment 1:
Utilize CVD system and device as shown in Figure 1, prepare the method for nitrogen-doped graphene at nonmetal substrate surface, described nonmetal substrate is silica/silicon substrate, mainly comprises the following steps:
In the 1st stage, first, the silicon substrate with 200-500 nano thickness silicon dioxide layer is put into sulfuric acid/hydrogen peroxide and carry out boiling half an hour, after taking-up, use successively deionized water, ethanol and acetone rinse repeatedly, and put into baking oven in 80 ℃ of oven dry, to remove as far as possible impurity on substrate surface.
The 2nd stage, the nonmetal substrate after cleaning is put into the high-temperature zone part of tubular type CVD system, in stove, pass into air, High Temperature Furnaces Heating Apparatus was heated to 800 ℃ in 20 minutes simultaneously, and under this state of temperature, keep 60 minutes, stop subsequently heating, furnace temperature is slowly reduced to room temperature.
The 3rd stage, first to the high-purity argon gas 30 minutes that passes into 500sccm in tubular type CVD system to drive as much as possible its inner air, subsequently argon flow amount is adjusted to 200sccm, and the hydrogen that passes into 50sccm is as carrier gas, and then High Temperature Furnaces Heating Apparatus is heated, make its temperature in 60 minutes, be elevated to 1100 ℃, and at this temperature, keep 20 minutes.
The 4th stage, at above-mentioned high-purity argon gas and hydrogen as carrier gas in the situation that, to passing into the methane of 10sccm and the ammonia of 20sccm in CVD system as carbon and nitrogen sources 120 minutes, stop subsequently passing into methane and ammonia, and stop heating, make temperature slowly be reduced to room temperature and then take out sample.
Be illustrated in figure 2 the present invention and at nonmetal substrate surface, prepare the process of growth schematic diagram of nitrogen-doped graphene.As shown in Figure 3, known by the analysis to Raman spectrogram, prepared nitrogen-doped graphene is minority layer structure to the Raman spectrum of the experiment sample that obtains, and has defect to a certain degree.This defect causes because nitrogen heteroatom doping enters graphene-structured inside.
Embodiment 2:
Press the preparation method of embodiment 1, change nonmetal silicon dioxide substrates into silicon nitride substrate, and this substrate can select not utilize sulfuric acid/hydrogen peroxide or liquid detergent, water, ethanol and acetone etc. to process its surface impurity, the nitrogen-doped graphene film obtaining is minority layer structure, and has higher homogeneity.
Embodiment 3:
Press the preparation method of embodiment 1, change nonmetal silicon dioxide substrates into Sapphire Substrate, and this substrate can select not utilize sulfuric acid/hydrogen peroxide or liquid detergent, water, ethanol and acetone etc. to process its surface impurity, the nitrogen-doped graphene film obtaining is minority layer structure, and has higher homogeneity.
Embodiment 4:
Press the preparation method of embodiment 1, nonmetal silicon dioxide substrates is changed into the substrate with curved surface or three-dimensional structure surface, the nitrogen-doped graphene film obtaining is minority layer structure, and has higher homogeneity.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. nonmetal substrate surface is prepared a method for nitrogen-doped graphene, it is characterized in that, comprises the following steps:
Step 1) is cleaned the surface of the nonmetal substrate with certain surface terrain feature;
Step 2) at described nonmetal substrate surface, prepare nitrogen-doped graphene film, mainly comprise the following steps:
201) the described nonmetal substrate cleaning up is put into the high-temperature zone part of tubular type CVD system;
202) furnace temperature was elevated between 600-1000 ℃ in 15-30 minute, and passes into air in this process, and reach after setting between 600-1000 ℃ of temperature and maintain 20-60 minute in furnace temperature, slowly reduce subsequently furnace temperature, make it reach room temperature;
203) furnace air is got rid of totally;
204) take hydrogen and high-purity argon gas as carrier gas in the situation that, within the time of 40-120 minute, furnace temperature is elevated between 1050-1500 ℃, and described nonmetal substrate is kept to 10-30 minute at this temperature;
205) pass into the growth of carrying out nitrogen-doped graphene containing the gas of carbon and nitrogen sources, and maintain 30-300 minute at 1050-1500 ℃ of temperature;
206) stop heating, furnace temperature is slowly reduced to room temperature.
2. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that, the concrete grammar of step 1 is as follows: described nonmetal substrate is placed in to sulfuric acid/hydrogen peroxide (70/30) solution and carries out boiling for some time; Or, first utilize liquid detergent repeatedly to wash by rubbing with the hands the nonmetal substrate of institute, put into successively respectively subsequently the tap water that is dissolved with liquid detergent, tap water, intermediate water, then takes out and dries at supersound process for some time in ethanolic soln and acetone soln from acetone soln; Or above-mentioned two kinds of methods are also used.
3. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that, the concrete grammar of step 203 is as follows: with vacuum pump, the pressure in described tubular type CVD system is controlled to the low-pressure state below 10mTorr, then be filled with high-purity argon gas to normal pressure, with vacuum pump, its pressure is reduced to below 10mTorr more subsequently, several times so repeatedly, to process the air in pipe as far as possible totally; Or, directly in described tubular type CVD system, pass into the high-purity argon gas 30 minutes of 500sccm to as far as possible furnace air is got rid of clean; Or above-mentioned two kinds of methods are also used.
4. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that furnace temperature is elevated between 1100-1300 ℃ in step 204.
5. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that, the gas containing carbon and nitrogen sources described in step 205 is methane and ammonia.
6. nonmetal substrate surface according to claim 5 is prepared the method for nitrogen-doped graphene, it is characterized in that, the flow that passes into of described methane is 1-30sccm; The flow that passes into of described ammonia is 10-50sccm.
7. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that: described nonmetal substrate is two dimensional structure, curved-surface structure or 3-D solid structure.
8. nonmetal substrate surface according to claim 1 is prepared the method for nitrogen-doped graphene, it is characterized in that: described nonmetal substrate is concave surface or the artificial metamaterial structure of convex mirror structure, optical grating construction, optical waveguide structure, photon crystal structure or fishing net shaped.
9. according to the nonmetal substrate surface described in claim 1 or 7 or 8, prepare the method for nitrogen-doped graphene, it is characterized in that: described nonmetal substrate is silicon base, silicon-dioxide substrate, the nitride silicon based end or sapphire substrates.
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Cited By (7)
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| CN103864064A (en) * | 2014-03-06 | 2014-06-18 | 新疆大学 | Method for preparing nitrogen-doped graphene |
| CN104495816A (en) * | 2014-12-12 | 2015-04-08 | 中国科学院重庆绿色智能技术研究院 | Fixture and method for preparing graphene by non-metal substrate intercalation-type nitrogen doping |
| CN108417781A (en) * | 2017-02-09 | 2018-08-17 | 硅力能股份有限公司 | Conducing composite material and its negative material and secondary cell of preparation |
| CN108609614A (en) * | 2018-05-28 | 2018-10-02 | 天津大学 | A kind of preparation method of blue, purple fluorescent single nitrogen-doped graphene |
| CN108878900A (en) * | 2018-06-20 | 2018-11-23 | 湖南国昶能源科技有限公司 | A kind of preparation method of the modified carbon felt of nitrogen-doped graphene |
| CN109928361A (en) * | 2019-03-19 | 2019-06-25 | 中国矿业大学 | A kind of carbon nanotube and hydrogen production system and method with self-catalysis function |
| CN110028058A (en) * | 2018-01-11 | 2019-07-19 | 北京石墨烯研究院 | A kind of nitrogen mixes grapheme material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864064A (en) * | 2014-03-06 | 2014-06-18 | 新疆大学 | Method for preparing nitrogen-doped graphene |
| CN104495816A (en) * | 2014-12-12 | 2015-04-08 | 中国科学院重庆绿色智能技术研究院 | Fixture and method for preparing graphene by non-metal substrate intercalation-type nitrogen doping |
| CN108417781A (en) * | 2017-02-09 | 2018-08-17 | 硅力能股份有限公司 | Conducing composite material and its negative material and secondary cell of preparation |
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| CN108609614A (en) * | 2018-05-28 | 2018-10-02 | 天津大学 | A kind of preparation method of blue, purple fluorescent single nitrogen-doped graphene |
| CN108878900A (en) * | 2018-06-20 | 2018-11-23 | 湖南国昶能源科技有限公司 | A kind of preparation method of the modified carbon felt of nitrogen-doped graphene |
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| CN109928361A (en) * | 2019-03-19 | 2019-06-25 | 中国矿业大学 | A kind of carbon nanotube and hydrogen production system and method with self-catalysis function |
| CN109928361B (en) * | 2019-03-19 | 2020-10-09 | 中国矿业大学 | Carbon nanotube and hydrogen production system and method with autocatalysis function |
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Application publication date: 20140122 |