CN113173578A - Nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and preparation method thereof - Google Patents
Nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and preparation method thereof Download PDFInfo
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- CN113173578A CN113173578A CN202110398294.8A CN202110398294A CN113173578A CN 113173578 A CN113173578 A CN 113173578A CN 202110398294 A CN202110398294 A CN 202110398294A CN 113173578 A CN113173578 A CN 113173578A
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/186—Preparation by chemical vapour deposition [CVD]
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Abstract
The invention discloses a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and a preparation method thereof. The preparation method has the advantages of simple preparation process, low energy consumption, low raw material cost and large-scale production; the nitrogen doped of the prepared nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial not only generates more defects and active centers on the surface of a carbon skeleton, but also effectively improves the electronic property and surface wettability of the carbon skeleton, and can be applied to a plurality of energy conversion and energy storage materials; and the used metal catalyst substrate can be completely removed, and the material cannot be polluted.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and a preparation method thereof.
Background
Carbon nanotubes and graphene belong to novel carbon nanomaterials, and have been sought by many researchers due to unique electrical, thermal, optical and mechanical properties. However, in the actual application process, the performance of the materials cannot be fully exerted, thereby greatly reducing the application range of the materials. This is mainly due to inevitable stacking or agglomeration caused by van der waals forces between graphite layers. In order to effectively solve this problem, a three-dimensional carbon material composed of graphene and carbon nanotubes has become a new round of research. In addition, the conductivity of the carbon nanomaterial is significantly changed by a hetero atom doping method. Particularly, nitrogen-doped carbon nano materials are very useful in the fields of future energy storage and new energy due to the unique electrochemical performance and stability of the nitrogen-doped carbon nano materials.
In recent years, three-dimensional carbon nanocomposites (carbon nanotube/graphene, carbon nanofiber/graphene, carbon nanotube/carbon nanofiber, etc.) have been receiving increasing attention. One aims to overcome the disadvantages of single carbon nanomaterials on one hand and to synergistically integrate materials of different dimensions by constructing three-dimensional nanostructures, thereby generating new physicochemical properties. The composite material often has a three-dimensional space network structure, and the unique morphology gives the composite material a wider application prospect. Compared with other synthesis methods, the CVD method can successfully prepare the three-dimensional carbon nano material with complete and intercommunicated structure without using toxic chemical reaction reagents and solutions polluting the environment.
The invention takes the cheap melamine as a single carbon nitrogen source, takes the nickel foam as a growth catalysis substrate, and grows the high nitrogen-doped carbon nano tube/graphene carbon nano material with a three-dimensional structure at a lower temperature of 800 ℃ by a one-step CVD method.
Disclosure of Invention
The invention aims to provide a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and a preparation method thereof, and the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial has the advantages of simple equipment, simplicity and convenience in operation, low energy consumption and the like.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial having a plurality of defects and active centers, thereby improving the electronic properties and surface wettability of the carbon backbone.
Preferably, the material is prepared by a CVD method from nickel foam and melamine, wherein the nickel foam is a catalyst substrate, and the melamine is a carbon nitrogen source.
The invention also provides a preparation method of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial, which comprises the following steps:
(1) nickel foam was mixed with melamine in a ratio of 1: 1-10, placing the mixture in a hydrogen atmosphere, heating to 600 ℃ according to a first heating rate, and then heating to 800 ℃ according to a second heating rate, wherein the first heating rate is greater than the second heating rate;
(2) then reacting for 0.5h at 800 ℃ in a mixed gas atmosphere, wherein the mixed gas comprises inert gas and hydrogen gas in a volume ratio of 5: 1.
Preferably, step (1) is preceded by a cleaning process, the cleaning process comprising the steps of: cutting the nickel foam into square blocks with the length of 10mm, immersing the square blocks in acetic acid for 10min by ultrasonic treatment, immersing the square blocks in ethanol for 10min by ultrasonic treatment, and finally blowing the residual acetic acid and ethanol on the surface of the nickel foam by nitrogen.
Preferably, step (3) is further included after step (2), and step (3) is specifically: cooled to room temperature under an inert gas atmosphere of 30 sccm.
Preferably, the first temperature rising rate in the step (1) is 30 ℃/min, and the second temperature rising rate is 20 ℃/min.
Preferably, the specific process of step (1) is as follows: nickel foam was mixed with melamine in a ratio of 1: 1-10, placing the mixture in a quartz boat in a tube furnace, introducing hydrogen, heating to 600 ℃ according to a first heating rate, and then heating to 800 ℃ according to a second heating rate.
Preferably, the inert gas in step (2) is argon or nitrogen.
Preferably, the specific process of step (2) is as follows: and (3) introducing inert gas and adjusting the flow rate of introduced hydrogen at the same time so that the flow rate ratio of the inert gas to the hydrogen is 5:1, and reacting for 0.5 h.
Preferably, the flow rate of the hydrogen in the step (1) is 70 sccm; the flow rate of the inert gas in the step (2) is 50 sccm.
The invention has the following beneficial effects:
(1) the preparation method has the advantages of simple preparation process, lower energy consumption, low raw material cost, lower synthesis temperature than that of the traditional CVD method for growing graphene by utilizing a gaseous carbon-nitrogen source, and large-scale production.
(2) The nitrogen-doped three-dimensional carbon nanotube/graphene material prepared by the invention not only generates more defects and active centers on the surface of the carbon skeleton, but also effectively improves the electronic property and the surface wettability of the carbon skeleton.
(3) The invention can control the sparseness and the uniformity of the carbon nano tube on the nitrogen-doped three-dimensional carbon nano tube/graphene carbon nano material by adjusting various experimental parameters such as the mass ratio of the carbon nitrogen source to the catalyst, the growth time and the like.
(4) The catalyst substrate used by the invention can be completely removed, and the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial cannot be polluted.
(5) The nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial obtained by the invention can be directly used for physical property detection and applied to various application related products.
Drawings
FIG. 1 is a schematic structural diagram of an experimental apparatus for preparing a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial according to the present invention;
fig. 2 is a Scanning Electron Microscope (SEM) image of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial prepared in example 1;
fig. 3 is a Scanning Electron Microscope (SEM) image of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial prepared in example 1;
fig. 4 is a Transmission Electron Microscope (TEM) image of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial prepared in example 1;
fig. 5 is a Scanning Electron Microscope (SEM) image of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial prepared in example 2;
fig. 6 is a Scanning Electron Microscope (SEM) image of the field emission of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial prepared in example 3;
fig. 7 is a field emission Scanning Electron Microscope (SEM) image of the carbon nanomaterial prepared in example 4.
Detailed Description
In order to further understand the present invention, the following describes a three-dimensional nitrogen-doped carbon nanotube/graphene carbon nanomaterial and a method for preparing the same according to the present invention with reference to examples.
The methods described in the following examples are conventional methods unless otherwise specified; the materials are commercially available, unless otherwise specified.
Example 1:
the experimental device for preparing the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in figure 1
1g of nickel foam was cut regularly to 10X 10mm2Clamping nickel foam by using a forceps, placing the nickel foam into acetic acid until the nickel foam is completely immersed, performing ultrasonic treatment in an ultrasonic instrument for 10 minutes, then immersing the nickel foam into ethanol, performing continuous ultrasonic treatment for 10 minutes, finally drying the residual acetic acid and ethanol on the surface of the nickel foam by using nitrogen, and taking the cleaned nickel foam as a catalyst substrate; melamine is used as a carbon-nitrogen source (precursor), 5g of melamine is mixed with 1g of pretreated nickel foam, then the mixture is placed on a quartz boat, the quartz boat is sent into a horizontal quartz tube with the outer diameter of 30mm and the inner diameter of 22mm of a CVD tubular furnace, 70sccm hydrogen (99.99%) is introduced into the CVD tubular furnace, the CVD tubular furnace is heated from room temperature to 600 ℃ at the heating rate of 30 ℃/min, then the heating rate is changed to 800 ℃ at the constant-temperature growth temperature at 20 ℃/min, the CVD tubular furnace is kept at 800 ℃, 50sccm argon is introduced at the same time, the hydrogen flow is adjusted to 10sccm, and after the constant-temperature growth is carried out for 0.5h, the operation is stoppedStopping introducing hydrogen, cooling the CVD tube furnace to room temperature under the atmosphere of 30sccm argon, and finally obtaining a black product in the quartz boat; the black product was placed in 3mol/L HCl solution at 80 ℃ for two days to completely remove the nickel foam substrate.
The SEM image of the obtained nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in fig. 2, the TEM image is shown in fig. 4, the SEM image of the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial after the nickel foam substrate is removed is shown in fig. 3, the nitrogen content of the material is up to 12.37% through XPS measurement, and more defects and active centers are generated on the surface of the carbon skeleton, thereby effectively improving the electronic properties and surface wettability of the carbon skeleton.
Example 2:
the experimental device for preparing the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in figure 1
1g of nickel foam was cut regularly to 10X 10mm2Clamping nickel foam by using a forceps, placing the nickel foam into acetic acid until the nickel foam is completely immersed, performing ultrasonic treatment in an ultrasonic instrument for 10 minutes, then immersing the nickel foam into ethanol, performing continuous ultrasonic treatment for 10 minutes, finally drying the residual acetic acid and ethanol on the surface of the nickel foam by using nitrogen, and taking the cleaned nickel foam as a catalyst substrate; melamine is used as a carbon-nitrogen source (precursor), 1g of melamine is mixed with 1g of pretreated nickel foam, then the mixture is placed on a quartz boat, the quartz boat is sent into a horizontal quartz tube with the outer diameter of 30mm and the inner diameter of 22mm of a CVD tubular furnace, 70sccm hydrogen (99.99%) is introduced into the CVD tubular furnace, the CVD tubular furnace is heated from room temperature to 600 ℃ at the heating rate of 30 ℃/min, then the heating rate is changed to 800 ℃ at the constant-temperature growth temperature at 20 ℃/min, the CVD tubular furnace is kept at 800 ℃, 50sccm argon is introduced at the same time, the hydrogen flow is adjusted to 10sccm, the introduction of hydrogen is stopped after the constant-temperature growth is carried out for 0.5h, the CVD tubular furnace is cooled to room temperature under the atmosphere of 30sccm argon, and finally a black product is obtained in the quartz boat; the black product was placed in 3mol/L HCl solution at 80 ℃ for two days to completely remove the nickel foam substrate.
The SEM image of the obtained nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in FIG. 5, more defects and active centers are generated on the surface of the carbon skeleton, and the electronic property and the surface wettability of the carbon skeleton are effectively improved.
Example 3:
the experimental device for preparing the nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in figure 1
1g of nickel foam was cut regularly to 10X 10mm2Clamping nickel foam by using a forceps, placing the nickel foam into acetic acid until the nickel foam is completely immersed, performing ultrasonic treatment in an ultrasonic instrument for 10 minutes, then immersing the nickel foam into ethanol, performing continuous ultrasonic treatment for 10 minutes, finally drying the residual acetic acid and ethanol on the surface of the nickel foam by using nitrogen, and taking the cleaned nickel foam as a catalyst substrate; melamine is used as a carbon-nitrogen source (precursor), 10g of melamine is mixed with 1g of pretreated nickel foam, then the mixture is placed on a quartz boat, the quartz boat is sent into a horizontal quartz tube with the outer diameter of 30mm and the inner diameter of 22mm of a CVD tubular furnace, meanwhile, 70sccm hydrogen (99.99%) is introduced, the temperature of the CVD tubular furnace is increased from room temperature to 600 ℃ at the temperature increase rate of 30 ℃/min, then the temperature increase rate is changed to 800 ℃ at the constant-temperature growth temperature at 20 ℃/min, the CVD tubular furnace is kept at 800 ℃, 50sccm argon is introduced at the same time, the hydrogen flow is adjusted to 10sccm, after the constant-temperature growth is carried out for 0.5h, the introduction of hydrogen is stopped, the CVD tubular furnace is cooled to room temperature under the atmosphere of 30sccm argon, and finally, a black product is obtained in the quartz boat; the black product was placed in 3mol/L HCl solution at 80 ℃ for two days to completely remove the nickel foam substrate.
The SEM image of the obtained nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is shown in FIG. 6, more defects and active centers are generated on the surface of the carbon skeleton, and the electronic property and the surface wettability of the carbon skeleton are effectively improved.
Example 4:
CVD tube furnace 400 ℃ and the experimental apparatus used is shown in FIG. 1
1g of nickel foam was cut regularly to 10X 10mm2Then clamping the nickel foam with a forceps, placing the nickel foam into acetic acid until the nickel foam is completely immersed, performing ultrasonic treatment in an ultrasonic instrument for 10 minutes, then immersing the nickel foam into ethanol, performing continuous ultrasonic treatment for 10 minutes, and finally blowing the residual acetic acid on the surface of the nickel foam by using nitrogen gasAnd ethanol, the cleaned nickel foam is used as a catalyst substrate; melamine is used as a carbon-nitrogen source (precursor), 1g of melamine is mixed with 1g of pretreated nickel foam, then the mixture is placed on a quartz boat, the quartz boat is sent into a horizontal quartz tube with the outer diameter of 30mm and the inner diameter of 22mm of a CVD tubular furnace, 70sccm hydrogen (99.99%) is introduced into the CVD tubular furnace, the CVD tubular furnace is heated from room temperature to 600 ℃ at the heating rate of 30 ℃/min, then the heating rate is changed to 800 ℃ at the constant-temperature growth temperature at 20 ℃/min, the CVD tubular furnace is kept at 400 ℃, 50sccm argon is introduced at the same time, the hydrogen flow is adjusted to 10sccm, the introduction of hydrogen is stopped after the constant-temperature growth is carried out for 0.5h, the CVD tubular furnace is cooled to room temperature under the atmosphere of 30sccm argon, and finally a black product is obtained in the quartz boat; the black product was placed in 3mol/L HCl solution at 80 ℃ for two days to completely remove the nickel foam substrate.
The SEM image of the obtained carbon nanomaterial is shown in fig. 7, and the nitrogen-doped carbon nanotube/graphene carbon nanomaterial with a three-dimensional structure is not grown.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is characterized in that the material has a plurality of defects and active centers.
2. The material of claim 1, wherein the material is prepared by CVD from nickel foam, which is a catalyst substrate, and melamine, which is a carbon nitrogen source.
3. A preparation method of a nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial is characterized by comprising the following steps:
(1) nickel foam was mixed with melamine in a ratio of 1: 1-10, placing the mixture in a hydrogen atmosphere, heating to 600 ℃ according to a first heating rate, and then heating to 800 ℃ according to a second heating rate, wherein the first heating rate is greater than the second heating rate;
(2) then reacting for 0.5h at 800 ℃ in a mixed gas atmosphere, wherein the mixed gas comprises inert gas and hydrogen gas in a volume ratio of 5: 1.
4. The method of claim 3, further comprising a cleaning process before the step (1), the cleaning process comprising the steps of: cutting the nickel foam into square blocks with the length of 10mm, immersing the square blocks in acetic acid for 10min by ultrasonic treatment, immersing the square blocks in ethanol for 10min by ultrasonic treatment, and finally blowing the residual acetic acid and ethanol on the surface of the nickel foam by nitrogen.
5. The preparation method according to claim 3, characterized by further comprising a step (3) after the step (2), wherein the step (3) is specifically: cooled to room temperature under an inert gas atmosphere of 30 sccm.
6. The production method according to claim 3, wherein the first temperature increase rate in step (1) is 30 ℃/min and the second temperature increase rate is 20 ℃/min.
7. The preparation method according to claim 3, wherein the specific process of the step (1) is as follows: nickel foam was mixed with melamine in a ratio of 1: 1-10, placing the mixture in a quartz boat in a tube furnace, introducing hydrogen, heating to 600 ℃ according to a first heating rate, and then heating to 800 ℃ according to a second heating rate.
8. The method according to claim 3, wherein the inert gas in the step (2) is argon or nitrogen.
9. The preparation method according to claim 3, wherein the specific process of the step (2) is as follows: and (3) introducing inert gas and adjusting the flow rate of introduced hydrogen at the same time so that the flow rate ratio of the inert gas to the hydrogen is 5:1, and reacting for 0.5 h.
10. The production method according to claim 3, wherein the flow rate of the hydrogen gas in the step (1) is 70 sccm; the flow rate of the inert gas in the step (2) is 50 sccm.
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