CN113092482A - Method for nondestructive detection of graphene point defects - Google Patents
Method for nondestructive detection of graphene point defects Download PDFInfo
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- CN113092482A CN113092482A CN201911338592.7A CN201911338592A CN113092482A CN 113092482 A CN113092482 A CN 113092482A CN 201911338592 A CN201911338592 A CN 201911338592A CN 113092482 A CN113092482 A CN 113092482A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/88—Investigating the presence of flaws or contamination
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention provides a method for nondestructive detection of graphene point defects, which is characterized in that graphene is covered on the surface of a metal foil by using methods such as chemical vapor deposition and the like, and is slowly baked in an oxygen-containing atmosphere at high temperature, so that copper under the defects is oxidized, and different contrasts can be seen under an optical microscope. According to the method provided by the invention, the point defects in the graphene can be observed under an optical microscope through very simple operation.
Description
Technical Field
The invention relates to a method for nondestructively detecting graphene point defects.
Background
At present, the research on the graphene defects is mainly to directly observe the atomic structure at the defects through microscopic techniques with atomic resolution, such as a Transmission Electron Microscope (TEM), a Scanning Tunneling Microscope (STM) and the like; the spatial distribution information of different crystal faces of the graphene can be obtained through a TEM dark field imaging mode and low-energy electron diffraction imaging (LEEM). The methods depend on a high-resolution imaging technology, have strong dependence on instruments, are complex to operate, have a detection area in a nanometer-micrometer order, and cannot realize rapid and large-area defect detection. In recent years, researchers can observe defects in graphene or distinguish crystal planes with different orientations to a certain extent by adding oxides, ultraviolet irradiation, spin coating liquid crystal display and the like. However, such methods by oxidation or molecular deposition reduce the quality of graphene to a greater or lesser extent. Therefore, a technique for rapidly and nondestructively detecting defects in graphene is important.
Disclosure of Invention
The invention provides a method for rapidly and nondestructively detecting point defects of graphene, wherein the graphene covers a metal foil and is slowly baked in a baking device for 1-40 hours. The metal foil includes copper foil, nickel foil, etc., preferably copper foil. The baking process is carried out in baking devices such as a hot table, an oven or a CVD tube furnace, and the like, and the temperature is set to be 100-300 ℃.
In the method provided by the invention, oxygen permeates at the point defect of the graphene under the low-temperature condition and oxidizes copper under the defect, so that the contrast of the defect can be seen under an optical microscope. According to the method provided by the invention, the point defects in the graphene can be observed under an optical microscope through very simple operation.
The invention provides a method for nondestructive detection of graphene point defects, which comprises the step of slowly baking graphene on a metal foil in a baking device to realize optical visualization of the point defects in the graphene.
Preferably, the graphene is grown on the metal foil by chemical vapor deposition, or is covered on the surface of the metal foil by means of transfer.
Preferably, the metal foil includes a copper foil or a nickel foil.
Preferably, the metal foil is a copper foil.
Preferably, the baking is carried out in the following gas atmosphere: air, a mixed gas containing oxygen, or a mixed gas containing oxygen and water vapor.
Preferably, the baking apparatus is a hot plate, an oven, or a CVD tube furnace.
Preferably, the point defect in the graphene can be observed by using an optical microscope.
Preferably, the method comprises the steps of:
growing graphene on the surface of a metal foil by using a normal-pressure chemical vapor deposition method;
secondly, slowly baking the metal foil sample covered with the graphene at low temperature;
and thirdly, directly observing the oxidized sample to see the point defects in the graphene.
Preferably, the method comprises the steps of:
growing graphene on the surface of a metal foil by using a normal-pressure chemical vapor deposition method;
slowly baking the metal foil sample covered with the graphene in a baking device for 1-100 hours at the baking temperature of 100-300 ℃;
and thirdly, directly observing the oxidized sample by using an optical microscope to see the point defects in the graphene.
The invention has the advantages that:
1. the invention relates to a method for nondestructive detection of graphene point defects;
2. the method utilizes a common heating table, an oven, a CVD tube furnace and the like to slowly and mildly oxidize the graphene on the copper foil, and is simple and convenient to operate;
3. the method can observe the point defects in the graphene under an optical microscope;
4. the method provided by the invention can keep the excellent performance of the graphene and has no damage to the graphene.
Drawings
FIG. 1 is a schematic diagram of a graphene sample covered on a copper foil, and the sample is annealed at 100-300 ℃ for 1-40 h to realize visualization of graphene point defects.
FIG. 2 (a) is an optical image of a graphene sample covered on a copper foil after annealing in air at 200 ℃ for 1 hour; fig. 2 (b) shows that the graphene sample covered on the copper foil is annealed in air at 200 ℃ for 100 hours, and graphene point defects can be seen through an optical microscope.
Fig. 3 shows raman spectrum results of graphene samples grown on copper foil before and after annealing. The Raman result shows that the treated graphene has no D peak corresponding to the defect, which shows that the treatment mode has little damage to the graphene.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are commercially available from the public unless otherwise specified.
The first embodiment is as follows: a method for rapidly and nondestructively detecting point defects and line defects of graphene comprises the following steps:
preparing graphene on the surface of a metal foil;
secondly, placing the metal foil sample covered with the graphene in a heating device, and annealing for 1-100 hours at 100-300 ℃;
and thirdly, after the annealing of the sample is finished, directly observing the sample by using an optical microscope to see the point defects in the graphene.
In the first step, graphene is grown on the metal foil by a chemical vapor deposition method, or is covered on the surface of the metal foil by a transfer mode. The metal foil includes copper foil, nickel foil, etc., preferably copper foil. The heating device comprises a heating table, an oven, a CVD tube furnace and the like. In a specific embodiment, the baking is performed in the following gas atmosphere: air, a mixed gas containing oxygen and/or water vapor.
In a specific embodiment, the prepared copper foil covered with graphene is annealed in air at 200 ℃ for 1h, and no graphene point defect occurs, as shown in fig. 2 (a); after annealing at 200 ℃ for 100 h in air, the appearance of graphene point defects can be seen under an optical microscope, as shown in fig. 2 (b). The results of the raman characterization of the graphene samples on the copper foil before and after annealing show that the quality of the graphene is hardly affected, as shown in fig. 3.
Test one: the method for nondestructively detecting the graphene point defects in the test is carried out according to the following steps:
growing graphene on the surface of a copper foil by using a normal-pressure chemical vapor deposition method;
secondly, placing the graphene sample on the copper foil in an oven, and annealing for 100 hours in the air at 130 ℃;
and thirdly, after the annealing of the sample is finished, directly observing the sample by using an optical microscope to see the point defects of the graphene.
Under the test condition, oxygen in the air is easy to permeate at the point defect, the copper at the lower layer is oxidized, and the optical contrast is changed, so that the point defect can be observed.
And (2) test II: the method for nondestructively detecting the graphene point defects in the test is carried out according to the following steps:
growing graphene on the surface of a nickel foil by using a normal-pressure chemical vapor deposition method;
secondly, placing the graphene sample on the copper foil on a hot table, and annealing for 20 hours in the air at 150 ℃;
and thirdly, after the annealing of the sample is finished, directly observing the sample by using an optical microscope to see the point defects of the graphene.
Under the test conditions, oxygen in the air is easy to permeate at the point defect, the copper at the lower layer is oxidized, and the optical contrast is changed, so that the copper can be observed.
And (3) test III: the method for nondestructively detecting the graphene point defects in the test is carried out according to the following steps:
growing graphene on the surface of a nickel foil by using a normal-pressure chemical vapor deposition method;
placing the graphene sample on the copper foil in a CVD (chemical vapor deposition) tube furnace, introducing protective gas (argon or nitrogen and the like) and oxygen with the volume percentage of 1-99%, and annealing for 100 hours at 100 ℃;
and thirdly, directly observing the sample by using an optical microscope after the annealing of the sample is finished, and then observing the point defects of the graphene crystal.
In step two, there may be no shielding gas, i.e. 100% oxygen.
Under the test condition, the introduced oxygen is easy to permeate at the point defect position, the copper at the lower layer is oxidized, and the optical contrast is changed, so that the copper can be observed.
And (4) testing: the method for nondestructively detecting the graphene point defects in the test is carried out according to the following steps:
firstly, covering graphene on the surface of a nickel foil in a transfer mode;
placing the graphene sample on the copper foil in a CVD (chemical vapor deposition) tube furnace, introducing protective gas (argon or nitrogen and the like) and oxygen and water vapor with the volume percentage of 1-99%, and annealing for 1 hour at 300 ℃;
and thirdly, after the annealing of the sample is finished, directly observing the sample by using an optical microscope to see the point defects of the graphene.
Under the test condition, the introduced oxygen and water vapor are easy to permeate at the point defect of the graphene, the copper at the lower layer is oxidized, and the optical contrast is changed, so that the copper can be observed.
And (5) testing: the method for nondestructively detecting the graphene point defects in the test is carried out according to the following steps:
firstly, covering graphene on the surface of a nickel foil in a transfer mode;
placing the graphene sample on the copper foil in a CVD (chemical vapor deposition) tube furnace, introducing protective gas (argon or nitrogen and the like) and water vapor with the volume percentage of 1-99%, and annealing for 1 hour at 300 ℃;
and thirdly, after the annealing of the sample is finished, directly observing the sample by using an optical microscope to see the point defects of the graphene.
Under the test condition, the introduced oxygen and water vapor are easy to permeate at the point defect of the graphene, the copper at the lower layer is oxidized, and the optical contrast is changed, so that the copper can be observed.
In the methods of the above-mentioned first to fifth experiments, it can be seen that the graphene point defects can be observed on the metal foil whether oxidized in the atmosphere, oxidized in the protective gas atmosphere containing oxygen, or oxidized in the protective atmosphere containing oxygen and water vapor.
Claims (10)
1. The method for nondestructively detecting the point defect of the graphene is characterized in that the graphene on a metal foil is slowly baked in a baking device to realize the optical visualization of the point defect of the graphene.
2. The method of claim 1, wherein the graphene is grown on the metal foil by chemical vapor deposition or covered on the surface of the metal foil by transfer.
3. The method of claim 2, wherein the metal foil comprises a copper foil or a nickel foil.
4. The method of claim 3, wherein the metal foil is copper foil.
5. The method of claim 1, wherein the baking is performed in a gas atmosphere comprising: air, a mixed gas containing oxygen, or a mixed gas containing oxygen and water vapor.
6. The method of claim 1, wherein the baking apparatus is a hot plate, an oven, or a CVD tube furnace.
7. The method of claim 1, wherein the point defects in the graphene are observable using an optical microscope.
8. The method according to any of claims 1-7, characterized in that the method comprises the steps of:
growing graphene on the surface of a metal foil by using a normal-pressure chemical vapor deposition method;
secondly, slowly baking the metal foil sample covered with the graphene at low temperature;
and thirdly, directly observing the oxidized sample to see the point defects in the graphene.
9. The method according to claim 8, characterized in that it comprises the steps of:
growing graphene on the surface of a metal foil by using a normal-pressure chemical vapor deposition method;
slowly baking the metal foil sample covered with the graphene in a baking device for 1-100 hours at the baking temperature of 100-300 ℃;
and thirdly, directly observing the oxidized sample by using an optical microscope to see the point defects in the graphene.
10. The method of claim 1, wherein the baking is performed in a mixture of a protective gas, oxygen and water vapor, wherein the oxygen comprises 1% to 98% by volume of the mixture, the water vapor comprises 1% to 98% by volume of the mixture, and the remainder is the protective gas.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749291A (en) * | 2012-07-12 | 2012-10-24 | 北京大学 | Optical microscope based method for detecting graphene quality |
| CN103352210A (en) * | 2013-06-24 | 2013-10-16 | 中国科学院上海微系统与信息技术研究所 | Method for visually displaying distribution of CVD (Chemical Vapor Deposition) graphene surface defects on metal substrate |
| CN104568554A (en) * | 2014-12-31 | 2015-04-29 | 泰州巨纳新能源有限公司 | Method for observing nucleation and growth of graphene on surface of metal base |
| CN106276873A (en) * | 2016-08-08 | 2017-01-04 | 中国科学院上海微系统与信息技术研究所 | A kind of method preparing germanio grapheme nano-pore |
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- 2019-12-23 CN CN201911338592.7A patent/CN113092482A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749291A (en) * | 2012-07-12 | 2012-10-24 | 北京大学 | Optical microscope based method for detecting graphene quality |
| CN103352210A (en) * | 2013-06-24 | 2013-10-16 | 中国科学院上海微系统与信息技术研究所 | Method for visually displaying distribution of CVD (Chemical Vapor Deposition) graphene surface defects on metal substrate |
| CN104568554A (en) * | 2014-12-31 | 2015-04-29 | 泰州巨纳新能源有限公司 | Method for observing nucleation and growth of graphene on surface of metal base |
| CN106276873A (en) * | 2016-08-08 | 2017-01-04 | 中国科学院上海微系统与信息技术研究所 | A kind of method preparing germanio grapheme nano-pore |
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