CN116654915A - Method for preparing vertical graphene array by taking foamy copper as catalyst - Google Patents
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- CN116654915A CN116654915A CN202310596476.5A CN202310596476A CN116654915A CN 116654915 A CN116654915 A CN 116654915A CN 202310596476 A CN202310596476 A CN 202310596476A CN 116654915 A CN116654915 A CN 116654915A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 64
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 58
- 239000010949 copper Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 239000006260 foam Substances 0.000 claims description 33
- 239000004744 fabric Substances 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 102000020897 Formins Human genes 0.000 claims description 4
- 108091022623 Formins Proteins 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims 1
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- -1 biosensors Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
Abstract
The application relates to a method for preparing a vertical graphene array by taking foamy copper as a catalyst, which comprises the following steps: s1, placing a substrate on the surface of the foamy copper, and then placing the foamy copper with the substrate placed in a reaction cavity of a Plasma Enhanced Chemical Vapor Deposition (PECVD) system; s2, vacuumizing a reaction cavity of the PECVD system, and introducing argon gas into the PECVD system after the vacuum degree reaches the requirement to create an inert gas atmosphere; s3, heating the temperature of the reaction cavity to 600-800 ℃ at a set heating rate, then introducing a set amount of carbon source, opening plasma for irradiation, and reacting at constant temperature for 1-2 hours; and S4, after the constant-temperature reaction is finished, closing the carbon source and the plasma, and cooling to obtain the vertical graphene array. The method is favorable for preparing the high-quality vertical graphene array rapidly and efficiently at low temperature.
Description
Technical Field
The application relates to the technical field of preparation of three-dimensional nano carbon materials, in particular to a method for preparing a vertical graphene array by taking foamy copper as a catalyst.
Background
In the last decade, the research of graphene has seen explosive growth. Graphene is a material composed of carbon atoms and sp 2 Two-dimensional materials with hexagonal honeycomb lattice composed of hybrid orbitals, whose lamellae form delocalized large pi bonds, electrons can move freely within them, thus exhibiting many excellent properties such as high transparency (97.7%), electron conductivity (106S cm) -1 ) Mechanical strength (1.1 TPa), thermal conductivity (5300W m) -1 K -1 ) Structural stability and specific surface area (2600 m) 2 g -1 ) Etc. In view of the unique and excellent properties of graphene, graphene is a candidate material for wide application, and has potential application in various fields such as catalysts, biosensors, composite materials, energy storage devices (lithium ion batteries, lithium sulfur batteries, zinc ion batteries, solar batteries and the like).
However, due to the influence of Van der Waals force, graphene crystal domains are easy to stack in the process of mutually splicing and continuously forming films, so that the specific surface area of graphene is greatly reduced, and the electrical performance of the graphene is reduced. Therefore, three-dimensionalization of graphene is a current major research hotspot. Compared with horizontally stacked graphene, the vertically aligned graphene array can effectively exert excellent performances such as high thermal conductivity, carrier mobility and the like of single graphene sheets. And secondly, the channel between graphene sheets effectively reduces the transmission obstruction of ions, molecules and the like in the vertical direction, shortens the transmission distance, has relatively large specific surface area and rich edges, and enhances the interaction between the graphene sheets and the external environment.
Along with the wide attention of researchers in various fields, the preparation method of the vertical graphene is also endless, such as a silicon carbide pyrolysis method, a 'flattening to straight' method by utilizing the original horizontally stacked graphene, a plasma chemical vapor deposition method and the like. One important advantage of plasma chemical vapor deposition (PECVD) is that the growth temperature of graphene can be significantly reduced and high quality vertical graphene can be produced.The main principle of PECVD for preparing vertical graphene is to bombard carbon source molecules (such as CH) by using high-energy electrons in plasma 4 、C 2 H 2 Etc.), the free carbon active particles are decomposed at a lower temperature, and the carbon active particles can form a flaky graphene structure on the surface of the substrate reaching a certain temperature. Therefore, due to the introduction of the plasma, not only pyrolysis of the carbon source gas by high temperature is avoided, but also the decomposition efficiency of the carbon source gas is greatly improved. The growth of vertical graphene using PECVD, while having the above-described advantages, is generally low in growth rate and difficult in growth control, because small variations in growth parameters may have a significant impact on the quality and structure of the graphene. In addition, vertical graphene grown by PECVD also has a problem in that the bonding with the substrate may be weak.
Disclosure of Invention
The application aims to provide a method for preparing a vertical graphene array by taking foamy copper as a catalyst, which is favorable for preparing the vertical graphene array with high quality rapidly, at low temperature and high efficiency.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows: a method for preparing a vertical graphene array by taking copper foam as a catalyst comprises the following steps:
s1, placing a substrate on the surface of the foamy copper, and then placing the foamy copper with the substrate placed in a reaction cavity of a Plasma Enhanced Chemical Vapor Deposition (PECVD) system;
s2, vacuumizing a reaction cavity of the PECVD system, and introducing argon gas into the PECVD system after the vacuum degree reaches the requirement to create an inert gas atmosphere;
s3, heating the temperature of the reaction cavity to 600-800 ℃ at a set heating rate, then introducing a set amount of carbon source, opening plasma for irradiation, and reacting at constant temperature for 1-2 hours;
and S4, after the constant-temperature reaction is finished, closing the carbon source and the plasma, and cooling to obtain the vertical graphene array.
Further, in step S1, before placing the substrate on the surface of the copper foam, the copper foam and the substrate were ultrasonically cleaned with acetone, absolute ethyl alcohol, and deionized water in this order for 30 minutes, and then dried in a vacuum oven at 60 ℃ for 2 hours.
Further, in step S1, the sizes of the copper foam and the substrate are 4 cm×3 cm, and the reaction chamber of the pecvd system is a quartz tube.
Further, the substrate is made of carbon cloth.
Further, the substrate is also made of copper foam, namely copper foam is used as the substrate and the catalyst at the same time, and the copper foam with a certain thickness is placed in a reaction cavity of a PECVD system to prepare the vertical graphene array.
Further, in the step S2, the requirement range of the vacuum degree is 1-10 Pa, and the flow rate of the introduced argon gas is 50-200 sccm; the pressure of the created inert gas atmosphere is 40-200 Pa.
Further, in step S3, the temperature rising rate is 10-30 ℃ for min -1 The flow rate of the carbon source is 10-50 sccm, and the power of the plasma is 80-150W.
Further, in step S3, the carbon source is methane or acetylene gas; the plasma is microwave, radio frequency or DC excited plasma.
In step S3, after the carbon source and the plasma are turned on, the vacuum degree of the reaction cavity is 60-300 Pa.
Further, in step S4, after the carbon source and the plasma are turned off, the carbon source and the plasma are cooled to below 100 ℃ to prepare the vertical graphene array.
Compared with the prior art, the application has the following beneficial effects: the method adopts the copper foam as the catalyst, the copper foam is a material with a highly porous structure and a large number of pores, wherein the pores are distributed in a microscopic level, and the structure enables the copper foam to have a larger specific surface area, provides more surface active sites and can promote the nucleation and growth of graphene. The substrate is placed on the surface of the foamy copper, and vertical graphene array growth is carried out on the surface of the substrate through plasma chemical vapor deposition, so that the growth speed is high, the low-temperature preparation is carried out, the process is simple, and the quality and the thickness of the grown graphene array are high and controllable. The vertical graphene array prepared by the method can meet the requirements of various fields such as catalysts, biosensors, composite materials, energy storage devices (lithium ion batteries, lithium sulfur batteries, zinc ion batteries, solar batteries and the like), and provides a new preparation method and research direction for scientific research and industrialization development in the fields.
Drawings
FIG. 1 is a schematic diagram of a method implementation of an embodiment of the present application.
Fig. 2 is a surface scanning electron microscope image of a carbon cloth/vertical graphene array in an embodiment of the present application.
Fig. 3 is a raman emission spectrum of a carbon cloth/vertical graphene array in an embodiment of the present application.
Fig. 4 is a surface scanning electron microscope image of a copper foam/vertical graphene array in an embodiment of the present application.
Detailed Description
The application will be further described with reference to the accompanying drawings and examples.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
As shown in fig. 1, the embodiment provides a method for preparing a vertical graphene array by using copper foam as a catalyst, which comprises the following steps:
s1, placing the substrate on the surface of the foamy copper, and then placing the foamy copper with the substrate placed in a reaction cavity of a Plasma Enhanced Chemical Vapor Deposition (PECVD) system.
And S2, vacuumizing a reaction cavity of the PECVD system, and introducing argon gas into the PECVD system after the vacuum degree reaches the requirement to create an inert gas atmosphere.
And S3, heating the reaction cavity to 600-800 ℃ at a set heating rate, then introducing a set amount of carbon source, opening plasma for irradiation, and reacting at constant temperature for 1-2 hours.
And S4, after the constant-temperature reaction is finished, closing the carbon source and the plasma, and cooling to obtain the vertical graphene array.
In this example, in step S1, the copper foam and the substrate were ultrasonically cleaned with acetone, absolute ethanol and deionized water in this order for 30 minutes before the substrate was placed on the surface of the copper foam, and then dried in a vacuum oven at 60 ℃ for 2 hours. The sizes of the foam copper and the substrate are 4 cm x 3 cm, and the reaction cavity of the PECVD system is a quartz tube.
In the preferred embodiment of the application, the substrate can be carbon cloth or copper foam, namely copper foam is used as the substrate and the catalyst at the same time, and the copper foam with the thickness larger than a set value is placed in a reaction cavity of a PECVD system to prepare the vertical graphene array.
In this embodiment, in step S2, the vacuum degree is required to be 1-10 Pa, and the flow rate of the introduced argon gas is 50-200 sccm. The pressure of the created inert gas atmosphere is 40-200 Pa.
In this embodiment, in step S3, the temperature rising rate is 10 to 30℃for min -1 The flow rate of the carbon source is 10-50 sccm, and the power of the plasma is 80-150W. The carbon source may be of the type methane or acetylene gas. The plasma includes microwave, radio frequency or direct current excited plasma. After the carbon source and the plasma are turned on, the vacuum degree of the reaction cavity is 60-300 Pa.
In this embodiment, in step S4, after the carbon source and the plasma are turned off, the vertical graphene array is prepared by cooling to below 100 ℃.
The experimental apparatus and reagents used in this example are commercially available.
Further description will be made with reference to several specific examples.
Example 1:
preparing a vertical graphene array by using 0.5 mm thick foamy copper and commercial carbon cloth as a catalyst and a substrate respectively, wherein the method comprises the following steps of:
(1) Copper foam having a thickness of 0.5. 0.5 mm was folded into a rectangular parallelepiped shape of 4 cm ×3 cm ×1 cm (length×width×height);
(2) Cutting commercial carbon cloth to a size of 4 cm ×3 cm and placing on the surface of copper foam (copper foam/carbon cloth);
(3) Disposing the copper/carbon foam in a reaction chamber (quartz tube) and then evacuating the quartz tube to about 2 Pa;
(4) Then introducing argon gas of 100 sccm into the quartz tube to create an inert atmosphere;
(5) After the air pressure is stabilized, the temperature is 10 ℃ for min -1 To 600 c and constant temperature 2 h at this temperature. Simultaneously, when the temperature is just raised to 600 ℃, the radio frequency plasma is immediately started, the power is set to be 80W, and 10 sccm of CH is introduced 4 The gas pressure was 60 Pa, and plasma and CH were turned off at the end of constant temperature 4 A gas;
(6) Cooling along with a furnace with Ar flow of 100 sccm to obtain a carbon cloth/vertical graphene nano-sheet array;
the scanning electron microscope and raman diffraction patterns of the carbon cloth/vertical graphene nanoplatelet array obtained in the embodiment are shown in fig. 2 and 3. As can be seen from fig. 2 and 3, the vertical graphene nanoplatelets are dense and uniform and have uniform dimensions. Raman spectra thereof are 1345, 1595 and 2676 cm respectively -1 Typical D, G and 2D peaks are shown here, which are typical features of graphite structures.
Example 2:
the method for preparing the vertical graphene array by directly and simultaneously taking 1 mm thick foam copper as a catalyst and a substrate comprises the following steps of:
(1) Copper foam having a thickness of 1 mm was folded into a rectangular parallelepiped shape of 8 cm ×3× 3 cm ×1× 1 cm (length×width×height);
(2) Placing the copper foam into a reaction chamber (quartz tube), and vacuumizing the quartz tube to about 5 Pa;
(3) Then introducing argon gas of 100 sccm into the quartz tube to create an inert atmosphere;
(4) After the air pressure is stabilized, the temperature is 10 ℃ for min -1 To 600 c and constant temperature 2 h at this temperature. Simultaneously, when the temperature is just raised to 600 ℃, the radio frequency plasma is immediately started, the power is set to be 80W, and 10 sccm of CH is introduced 4 The gas pressure was 60 Pa, and plasma and CH were turned off at the end of constant temperature 4 A gas;
(5) Cooling along with a furnace with Ar flow of 100 sccm to obtain a foam copper/vertical graphene nano-sheet array;
a scanning electron microscope image of the foamy copper/vertical graphene nano-sheet array obtained in the embodiment is shown in fig. 4.
The above description is only a preferred embodiment of the present application, and is not intended to limit the application in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present application still fall within the protection scope of the technical solution of the present application.
Claims (10)
1. The method for preparing the vertical graphene array by taking the foamy copper as the catalyst is characterized by comprising the following steps of:
s1, placing a substrate on the surface of the foamy copper, and then placing the foamy copper with the substrate placed in a reaction cavity of a Plasma Enhanced Chemical Vapor Deposition (PECVD) system;
s2, vacuumizing a reaction cavity of the PECVD system, and introducing argon gas into the PECVD system after the vacuum degree reaches the requirement to create an inert gas atmosphere;
s3, heating the temperature of the reaction cavity to 600-800 ℃ at a set heating rate, then introducing a set amount of carbon source, opening plasma for irradiation, and reacting at constant temperature for 1-2 hours;
and S4, after the constant-temperature reaction is finished, closing the carbon source and the plasma, and cooling to obtain the vertical graphene array.
2. The method for preparing a vertical graphene array using copper foam as a catalyst according to claim 1, wherein in step S1, the copper foam and the substrate are sequentially ultrasonically cleaned with acetone, absolute ethyl alcohol and deionized water for 30 minutes before being placed on the surface of the copper foam, and then dried in a vacuum drying oven at 60 ℃ for 2 hours.
3. The method for preparing the vertical graphene array by using the foamy copper as the catalyst according to claim 1, wherein in the step S1, the foamy copper and the substrate are both 4 cm by 3 cm in size, and a reaction cavity of a PECVD system is a quartz tube.
4. The method for preparing the vertical graphene array by using the copper foam as the catalyst according to claim 1, wherein the substrate is carbon cloth.
5. The method for preparing the vertical graphene array by using the copper foam as the catalyst according to claim 1, wherein the copper foam is also adopted as the substrate, namely the copper foam is used as the substrate and the catalyst at the same time, and the copper foam with a certain thickness is placed in a reaction cavity of a PECVD system to prepare the vertical graphene array.
6. The method for preparing the vertical graphene array by using the foamy copper as the catalyst according to claim 1, wherein in the step S2, the vacuum degree is required to be 1-10 Pa, and the flow rate of the argon gas is 50-200 sccm; the pressure of the created inert gas atmosphere is 40-200 Pa.
7. The method for preparing a vertical graphene array by using foamy copper as a catalyst according to claim 1, wherein in the step S3, the heating rate is 10-30 ℃ for min -1 The flow rate of the carbon source is 10-50 sccm, and the power of the plasma is 80-150W.
8. The method for preparing a vertical graphene array by using foamy copper as a catalyst according to claim 1, wherein in the step S3, the carbon source is methane or acetylene gas; the plasma is microwave, radio frequency or DC excited plasma.
9. The method for preparing the vertical graphene array by using the foamy copper as the catalyst according to claim 1, wherein in the step S3, after the carbon source and the plasma are turned on, the vacuum degree of the reaction cavity is 60-300 Pa.
10. The method for preparing the vertical graphene array by using the foamy copper as the catalyst according to claim 1, wherein in the step S4, the vertical graphene array is prepared by cooling to below 100 ℃ after the carbon source and the plasma are turned off.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310596476.5A CN116654915A (en) | 2023-05-25 | 2023-05-25 | Method for preparing vertical graphene array by taking foamy copper as catalyst |
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| CN202310596476.5A CN116654915A (en) | 2023-05-25 | 2023-05-25 | Method for preparing vertical graphene array by taking foamy copper as catalyst |
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