CN108502873B - Preparation method of high-quality graphene with few defects and uniform structure - Google Patents
Preparation method of high-quality graphene with few defects and uniform structure Download PDFInfo
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Abstract
The invention designs a preparation method of graphene with high quality, few defects and uniform structure, which comprises the following steps: pretreating a catalyst nickel-plated carbon fiber; growing by adopting a PECVD method; setting corresponding technological parameters of an instrument for growth; and (5) after the growth is finished, closing all water, electricity and gas, and taking out a growth sample for characterization. According to the invention, nickel-plated carbon fibers are used as a catalyst, and the prepared graphene has the advantages of uniform structure, high quality and less impurities.
Description
Technical Field
The invention belongs to the field of graphene preparation, and particularly relates to a preparation method of high-quality graphene with few defects and a uniform structure.
Background
Graphene has a unique structure and excellent properties, and also has good flexibility and light transmission. The method has wide application prospect in the fields of electronics, information, energy, materials, biomedicine and the like. For better application of the novel material, how to controllably synthesize high-quality graphene is a difficulty which must be overcome. Chemical Vapor Deposition (CVD) has attracted much attention because it can grow large-area, high-quality, continuous graphene films, as compared to chemical redox, mechanical lift-off, and silicon carbide surface epitaxial growth. Based on the growth mechanism of graphene, the influence of the selection of the substrate on the CVD growth of graphene is also very large from the viewpoint of the selection of the substrate material.
CVD is one of the mainstream methods for preparing single crystal high quality graphene at present, and the method adopts a carbon-containing gas source such as methane, acetylene, ethylene and the like as a precursor, carbon source gas molecules are cracked at high temperature to generate carbon atoms, and the carbon atoms form nuclei on a metal substrate to gradually crystallize and form a film under the conditions of proper temperature, pressure and gas ratio. The transition metal of the catalyst commonly used at present comprises copper foil and nickel film. But the growth mechanism on copper and nickel is different. Deposition on nickel tends to be a carbon carburization mechanism, while on copper foil is a surface-limiting growth mechanism. For a metal matrix with high carbon dissolving amount of nickel, pyrolytic carbon atoms generated by pyrolysis of a carbon source precursor penetrate into the metal at high temperature to form a solid solution with nickel at high temperature, and the previous carbon is gradually separated out on the surface to form a nucleation and crystallization film with the reduction of the temperature. However, growth on nickel is not easy to adjust various parameters, resulting in high quality disorder of the grown film.
The nickel-plated carbon fiber belongs to the field of metal-based composite materials, is a novel high-strength and high-modulus material, and has good conductivity. The nickel-plated carbon fiber reinforced composite material has excellent rigidity and strength, smaller thermal expansion coefficient and specific gravity and better catalytic performance, so that the invention invents a method for preparing high-quality graphene with few defects and uniform structure by using a Plasma Enhanced Chemical Vapor Deposition (PECVD) method and taking a nickel-plated carbon fiber material as a catalyst by utilizing the advantages of nickel-plated carbon fibers.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of graphene with high quality, few defects and uniform structure, which adopts nickel-plated carbon fiber as a catalyst, methane as a carbon source and PECVD-based growth of graphene at a lower temperature.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of high-quality graphene with few defects and uniform structure comprises the following steps:
(1) cutting nickel-plated carbon fibers with the length of 10cm, soaking the nickel-plated carbon fibers in acetone for 2 hours, and completely removing a sizing agent on the nickel-plated carbon fibers, wherein the content of the carbon fiber sizing agent is 1.0-1.5%;
(2) opening the electricity, gas and tail gas absorption device; CH (CH)4、H2The Ar main switch, the first pressure reducing valve and the second pressure reducing valve;
(3) opening a PECVD power switch and an instrument switch, starting a vacuum detection unit switch, detecting the vacuum degree of the instrument, keeping the vacuum degree below 0.5Pa, testing the pressure maintaining effect, after testing by a vacuum system, cutting the nickel-plated carbon fiber on a 10cm long quartz boat, placing the boat on a heating zone of a quartz tube, and closing a furnace cavity door of a flange plate;
(4) vacuumizing: opening a baffle valve, closing a switch of a tail gas linkage device, and clicking a starting button of a vacuum system device until the pressure in the quartz tube is reduced to be below 0.5 Pa;
(5) heating: clicking a heating control unit operation button until the temperature rises to a target temperature;
(6) constant temperature annealing: opening H2Switching ON the air inlet switch, turning ON the mixed air inlet switch, clicking the automatic air inlet setting button, turning ON the plasma switch, adjusting the power to the target power, clicking the ON button of plasma, and after 30min, H2The flow is automatically closed;
(7) growing: open CH4Air inlet switch, click automatic air inlet setting button, H after 15min2Automatically closing the flow, adjusting the plasma power to the target power, adjusting the plasma power to 0W after the growth is finished, closing a plasma switch, and clicking an OFF button;
(8) cooling: opening an Ar air inlet switch, clicking an automatic air inlet setting button, and closing H2、CH4An air inlet is opened and closed, and the Ar flow is automatically closed after 50 min;
(9) cooling and sampling: when the temperature of the furnace body is reduced to 50 ℃, closing the vacuum detection unit, closing the Ar air inlet and the mixed air inlet switch, and opening the flange plate to take out the sample;
(10) shutdown: and closing the instrument button to an OFF gear and a LOCK switch, closing an instrument power switch and a power main switch, and closing all the gas circuit switch buttons.
Furthermore, the nickel plating thickness of the nickel-plated carbon fiber is 0.2-1.0mm, the surface is rough and uneven, and the diameter is about 8 mm.
Further, the target temperature is 750 ℃.
Further, the target power for PECVD is adjusted to 40W.
Further, H is constant temperature annealing2The flow rate of (2) is 10 sccm.
Further, H is grown2Flow rate of (2) is 5sccm, CH4The flow rate of (2) is 4 sccm.
Further, the flow rate of Ar is 50sccm when the temperature is reduced.
The invention has the beneficial effects that: the graphene prepared by the invention has the advantages of uniform structure, high quality, less impurities, lower reaction temperature, less energy consumption and shorter total reaction time.
Drawings
Fig. one is an SEM image of graphene grown on the nickel-plated carbon fiber prepared in example 1 of the present invention;
fig. two is a raman spectrum of graphene grown on the nickel-plated carbon fiber prepared in example 1 of the present invention;
fig. three is an SEM image of graphene grown on the nickel-plated carbon fiber prepared in example 2 of the present invention;
fig. four is a raman spectrum of graphene grown on the nickel-plated carbon fiber prepared in example 2 of the present invention;
FIG. V is an SEM image of graphene grown on the nickel-plated carbon fiber prepared in example 3 of the present invention;
fig. six is a raman spectrum of graphene grown on the nickel-plated carbon fiber prepared in example 3 of the present invention.
Detailed Description
Example 1
(1) Cutting nickel-plated carbon fibers with the length of 10cm, soaking the nickel-plated carbon fibers in acetone for 2 hours, and completely removing sizing agents on the nickel-plated carbon fibers, wherein the content of the sizing agents on the carbon fibers is 1.2%, and the content of the sizing agents on different sections of the same fiber is basically stable.
(2) Opening the electricity, gas and tail gas absorption device and CH4、H2The Ar switch main switch, the first pressure reducing valve and the second pressure reducing valve.
(3) And opening a power switch and an instrument switch of the Plasma Enhanced Chemical Vapor Deposition (PECVD), starting a vacuum detection unit switch, detecting the vacuum degree (below 0.5 Pa) and the pressure maintaining effect of the instrument, cutting the nickel-plated carbon fiber of the next figure into a heating area with a 10cm long quartz boat and a quartz tube, and closing the furnace cavity door of the flange plate after the vacuum system has no problem.
(4) Vacuumizing: and opening the baffle valve, closing a switch of the tail gas linkage device, and clicking a starting button of the vacuum system device until the pressure in the quartz tube is below 0.5 Pa.
(5) Setting technological parameters: target temperature: 700 ℃, temperature rise time: 50min, annealing time: 30min, H on annealing2Flow rate: 10sccm, annealing power: 40W, growth time: 30min, growth H2Flow rate: 5sccm, CH during growth4Flow rate: 4sccm, power during growth: and 40W, and the Ar flow rate is 50sccm during temperature reduction.
(6) Heating: clicking a heating control unit operation button until the temperature rises to a target temperature;
(7) constant temperature annealing: opening H2Switching ON the air inlet switch, turning ON the mixed air inlet switch, clicking the automatic air inlet setting button, turning ON the plasma switch, adjusting the power to the target power, clicking the ON button, and after 30min, H2The flow is automatically closed;
(8) growing: open CH4Air inlet switch, click automatic air inlet setting button, H after 15min2Automatically closing the flow, adjusting the plasma power to the target power, adjusting the plasma power to 0W after the growth is finished, closing a plasma switch, and clicking an OFF button;
(9) cooling: opening an Ar air inlet switch, clicking an automatic air inlet setting button, and closing H2、CH4An air inlet is opened and closed, and the Ar flow is automatically closed after 50 min;
(10) cooling and sampling: when the temperature of the furnace body is reduced to 50 ℃, closing the vacuum detection unit, closing the Ar air inlet and the mixed air inlet switch, opening the flange plate, and taking out the sample;
(11) shutdown: and closing the instrument button to an OFF gear and a LOCK switch, closing an instrument power switch and a power main switch, and closing all the gas circuit switch buttons.
And (3) growing results: the quartz tube wall is not blackened, and the nickel-plated carbon fiber surface is not obviously changed and is only slightly darker than the color before growth.
Example 2
(1) The above steps (1) to (4) are the same as in example 1.
(2) Setting technological parameters: target temperature: 750 ℃, temperature rise time: 55min, annealing time: 30min, H on annealing2Flow rate: 10sccm, annealing power: 40W, growth time: 30min, growth H2Flow rate: 5sccm, CH during growth4Flow rate: 4sccm, power during growth: and 40W, and the Ar flow rate is 50sccm during temperature reduction.
(3) The above-mentioned processes (6) to (11) are the same as those in example 1.
And (3) growing results: the quartz tube wall is not blackened, the nickel-plated carbon fiber surface is not obviously changed, and the color is slightly darker than that before growth.
Example 3
(1) The above steps (1) to (4) are the same as in example 1.
(2) Setting technological parameters: target temperature: temperature rise time at 800 ℃: 70min, annealing time: 30min, H on annealing2Flow rate: 10sccm, annealing power: 40W, growth time: 30min, growth H2Flow rate: 5sccm, CH during growth4Flow rate: 4sccm, power during growth: and 40W, and the Ar flow rate is 50sccm during temperature reduction.
(3) The above-mentioned processes (6) to (11) are the same as in example 1.
And (3) growing results: the wall of the quartz tube is blackened and blackened, the surface state of the nickel-plated carbon fiber is not obviously changed, and the color is slightly darker than that before growth.
Specific data of coverage degree, total process time, uniform structure and defect statistics of the graphene prepared in the embodiments 1 to 3 of the invention are shown in table 1. TABLE 1
Claims (6)
1. A preparation method of high-quality graphene with few defects and uniform structure is characterized by comprising the following steps:
(1) cutting nickel-plated carbon fibers with the length of 10cm, soaking the nickel-plated carbon fibers in acetone for 2 hours, and completely removing a sizing agent on the nickel-plated carbon fibers, wherein the content of the carbon fiber sizing agent is 1.0-1.5%;
(2) opening the electricity, gas and tail gas absorption device; CH (CH)4、H2The Ar main switch, the first pressure reducing valve and the second pressure reducing valve;
(3) opening a PECVD power switch and an instrument switch, starting a vacuum detection unit switch, detecting the vacuum degree of the instrument, keeping the vacuum degree below 0.5Pa, testing the pressure maintaining effect, after testing by a vacuum system, cutting the nickel-plated carbon fiber on a 10cm long quartz boat, placing the boat on a heating zone of a quartz tube, and closing a furnace cavity door of a flange plate;
(4) vacuumizing: opening a baffle valve, closing a switch of a tail gas linkage device, and clicking a starting button of a vacuum system device until the pressure in the quartz tube is reduced to be below 0.5 Pa;
(5) heating: clicking a heating control unit operation button until the temperature rises to a target temperature;
(6) constant temperature annealing: opening H2Switching ON the air inlet switch, turning ON the mixed air inlet switch, clicking the automatic air inlet setting button, turning ON the plasma switch, adjusting the power to the target power, clicking the ON button of plasma, and after 30min, H2The flow is automatically closed;
(7) growing: open CH4An air inlet switch, wherein an automatic air inlet setting button is clicked, the H2 flow is automatically closed after 15min, the plasma power is adjusted to the target power, after the growth is finished, the plasma power is adjusted to 0W, the plasma switch is closed, and an OFF button is clicked;
(8) cooling: opening an Ar air inlet switch, clicking an automatic air inlet setting button, and closing H2、CH4An air inlet is opened and closed, and the Ar flow is automatically closed after 50 min;
(9) cooling and sampling: when the temperature of the furnace body is reduced to 50 ℃, closing the vacuum detection unit, closing the Ar air inlet and the mixed air inlet switch, and opening the flange plate to take out the sample;
(10) shutdown: closing the instrument button to an OFF gear, a LOCK switch, an instrument power switch and a power main switch, and closing all gas circuit switch buttons;
the target temperature is 750 ℃;
annealing at constant temperature H2The flow rate of (2) is 10 sccm.
2. The method for preparing high-quality graphene with few defects and uniform structure according to claim 1, wherein the method comprises the following steps: the nickel plating thickness of the nickel-plated carbon fiber is 0.2-1.0mm, the surface is rough and uneven, and the diameter is 8 mm.
3. The method for preparing high-quality graphene with few defects and uniform structure according to claim 1, wherein the method comprises the following steps: the target power adjusted for PECVD is 40W.
4. The method for preparing high-quality graphene with few defects and uniform structure according to claim 1, wherein the method comprises the following steps: growth H2Flow rate of (2) is 5sccm, CH4The flow rate of (2) is 4 sccm.
5. The method for preparing high-quality graphene with few defects and uniform structure according to claim 1, wherein the method comprises the following steps: the Ar flow is 50sccm when the temperature is reduced.
6. The method for preparing high-quality graphene with few defects and uniform structure according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) cutting nickel-plated carbon fibers with the length of 10cm, soaking the nickel-plated carbon fibers in acetone for 2 hours, and completely removing sizing agents on the nickel-plated carbon fibers, wherein the content of the sizing agents on the carbon fibers is 1.2%, and the content of the sizing agents on different sections of the same fiber is basically stable;
(2) opening the electricity, gas and tail gas absorption device and CH4、H2The Ar switch main switch, the first pressure reducing valve and the second pressure reducing valve are arranged on the main switch;
(3) opening a power switch and an instrument switch of the plasma enhanced chemical vapor deposition, starting a vacuum detection unit switch, detecting the vacuum degree of the instrument to be less than 0.5Pa and the pressure maintaining effect, cutting the nickel-plated carbon fiber of the next figure into a 10cm long quartz boat and placing a heating area of a quartz tube after a vacuum system has no problem, and closing a furnace cavity door of a flange plate;
(4) vacuumizing: opening a baffle valve, closing a tail gas linkage device switch, and clicking a starting button of a vacuum system device until the pressure in the quartz tube is below 0.5 Pa;
(5) setting technological parameters: target temperature: 750 ℃, temperature rise time: 55min, annealing time: 30min, H on annealing2Flow rate: 10sccm, annealing power: 40W, growth time: 30min, growth H2Flow rate: 5sccm, CH during growth4Flow rate: 4sccm, power during growth: 40W, and the Ar flow is 50sccm during temperature reduction;
(6) heating: clicking a heating control unit operation button until the temperature rises to a target temperature;
(7) constant temperature annealing: opening H2Switching ON the air inlet switch, turning ON the mixed air inlet switch, clicking the automatic air inlet setting button, turning ON the plasma switch, adjusting the power to the target power, clicking the ON button, and after 30min, H2The flow is automatically closed;
(8) growing: open CH4Air inlet switch, click automatic air inlet setting button, H after 15min2Automatically closing the flow, adjusting the plasma power to the target power, adjusting the plasma power to 0W after the growth is finished, closing a plasma switch, and clicking an OFF button;
(9) cooling: opening an Ar air inlet switch, clicking an automatic air inlet setting button, and closing H2、CH4An air inlet is opened and closed, and the Ar flow is automatically closed after 50 min;
(10) cooling and sampling: when the temperature of the furnace body is reduced to 50 ℃, closing the vacuum detection unit, closing the Ar air inlet and the mixed air inlet switch, opening the flange plate, and taking out the sample;
(11) shutdown: and closing the instrument button to an OFF gear and a LOCK switch, closing an instrument power switch and a power main switch, and closing all the gas circuit switch buttons.
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| CN109763320B (en) * | 2018-12-24 | 2020-07-10 | 西安交通大学 | Process for repairing carbon fiber surface holes and cracks by graphene film |
| CN109824038B (en) * | 2019-02-20 | 2022-03-25 | 南京大学 | Method for efficiently eliminating graphene wrinkles by chemical vapor deposition |
| CN113072063B (en) * | 2020-07-10 | 2024-01-23 | 华南理工大学 | Hydrogen-resistant coating based on inner surface of hydrogen storage and transportation equipment and preparation method thereof |
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