CN112978711B - Method for transferring large-area graphite alkyne film - Google Patents
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- CN112978711B CN112978711B CN202110308552.9A CN202110308552A CN112978711B CN 112978711 B CN112978711 B CN 112978711B CN 202110308552 A CN202110308552 A CN 202110308552A CN 112978711 B CN112978711 B CN 112978711B
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Abstract
The invention discloses a method for transferring a graphite alkyne film in a large area, which relates to a material transfer process after a two-dimensional material grows and before a device is prepared, and comprises the following steps: uniformly coating polymethyl methacrylate on the graphite alkyne film on the copper foil which is subjected to the oxygen plasma reaction etching thinning, and placing the graphite alkyne film in a saturated ferric chloride solution for reaction etching; fishing out the graphite alkyne film attached with the polymethyl methacrylate from a saturated ferric chloride solution by using a clean silicon wafer, cleaning the graphite alkyne film in deionized water, and fishing out the graphite alkyne film again by using a target substrate; heating and drying by a hot plate, continuously heating to enable the graphite alkyne film to be tightly attached to a target substrate, placing the graphite alkyne film in an acetone solution to be heated and remove glue, fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the graphite alkyne film in an isopropanol solution for cleaning, fishing out the graphite alkyne film, and drying the graphite alkyne film by using nitrogen. The method is simple to operate, can easily realize the complete transfer of the graphite alkyne film on the copper foil, and the obtained graphite alkyne film is cleaner, thereby solving the problem that the graphite alkyne film is difficult to directionally transfer from the copper foil in a large area.
Description
Technical Field
The invention relates to a material transfer process after a two-dimensional material grows and before a device is prepared, in particular to a method for transferring a graphite alkyne film in a large area.
Background
Since 2010, the first research on a method for synthesizing large-area graphyne by the group of li-jade-well academicians, the two-dimensional semiconductor material graphyne has attracted much attention. The graphathic material having carbon at the same timeSp and sp of2Theoretical calculation shows that the hybrid has a proper forbidden band width (0.46-1.22 eV) and ultrahigh carrier mobility (hole transport mobility), so that the hybrid has a wide application prospect and obvious competitive advantages in the field of photoelectrons. However, the lack of a method for effectively transferring the synthesized graphyne film to a target substrate in a large area also limits the research and application of two-dimensional graphyne semiconductor materials in the fields of electronic devices and photoelectric devices to a certain extent. The realization and perfection of the large-area graphite alkyne film transfer process can promote the research and application of graphite alkyne semiconductor materials in the field of electronic and photoelectric device integration.
However, the position, size and shape of the graphite alkyne which can be transferred by the traditional method for synthesizing the two-dimensional graphite alkyne by wet transfer of the Glaser coupling reaction under the laboratory condition are uncontrollable, the area of the graphite alkyne on a generally obtained target substrate is small, and the construction of an electronic or photoelectric device is inconvenient, so that a large-area graphite alkyne film transfer method needs to be developed.
Disclosure of Invention
The invention aims to overcome the defects of the existing process, improve the process parameters of the existing wet transfer, and provide a method for transferring the graphite alkyne film in a large area in a laboratory.
According to the technical scheme of the invention, the method for transferring the graphite alkyne film in a large area is provided, and the method specifically comprises the following steps:
s1, uniformly coating polymethyl methacrylate on the graphite alkyne film on the copper foil which is thinned by the oxygen plasma reaction etching, and placing the graphite alkyne film in a saturated ferric chloride solution for reaction etching;
s2, fishing out the graphite alkyne film attached with the polymethyl methacrylate from the saturated ferric chloride solution by using a clean silicon wafer, cleaning the graphite alkyne film in deionized water, and fishing out the graphite alkyne film again by using a target substrate;
s3, heating and drying by a hot plate, then continuously heating to enable the graphite alkyne film to be tightly attached to a target substrate, finally placing the graphite alkyne film into an acetone solution to be heated and remove glue, fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the graphite alkyne film into an isopropanol solution to be cleaned, fishing out the graphite alkyne film, and drying the graphite alkyne film by using nitrogen.
Further, in step S1, the graphdiyne film is synthesized by Glaser alkyne coupling reaction using hexaethynylbenzene as a monomer on the copper foil.
Further, the thickness of the graphite alkyne film is 800-1000 nm.
Further, in step S2, the target substrate is surface SiO2A 300nm thick U.S. silicon wafer.
Further, the target substrate is about 300nm thick.
Further, step S1 is specifically: uniformly coating polymethyl methacrylate on the surface of the graphite alkyne film on the copper foil subjected to the oxygen plasma reaction etching thinning, scraping off clean graphite alkyne from the surface of the graphite alkyne film which is not coated, placing the copper foil on the surface of a saturated ferric chloride solution with the surface facing downwards, standing for 12 hours for reaction etching, and completely reacting the copper foil.
Further, step S2 is specifically: and fishing out the graphite alkyne film attached with the polymethyl methacrylate from the saturated ferric chloride solution by using a clean silicon wafer, putting the graphite alkyne film into deionized water for cleaning for 3-4 times, and finally fishing out the graphite alkyne film with the target substrate.
Further, in step S2, the surface to which the graphdiyne film is attached to a target substrate.
Further, step S3 is specifically: heating the graphite alkyne film by a hot plate for 40-60 ℃/5-7 min, then heating the graphite alkyne film for 180-250 ℃/3-6 min to enable the graphite alkyne film to be tightly attached to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating for 85-95 ℃/10-15 min to remove glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the acetone alkyne film in an isopropanol solution for cleaning, and then fishing out the graphite alkyne film and drying the graphite alkyne film by using nitrogen.
Further, step S3 is specifically: heating the graphite alkyne film on a hot plate at a speed of 50 ℃/5min for drying, then heating the graphite alkyne film at a speed of 250 ℃/5min for tightly adhering the graphite alkyne film to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating at a speed of 90 ℃/15min for removing glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the acetone alkyne film in an isopropanol solution for cleaning, fishing out the acetone alkyne film, and drying the acetone alkyne film by using nitrogen.
The beneficial results of the invention are as follows: aiming at the problem that large-area directional transfer of a two-dimensional graphite alkyne material is difficult, the traditional wet transfer method is improved by low-temperature drying and high-temperature heating, so that the graphite alkyne separated from the copper foil is completely transferred to a target substrate, a plurality of points are taken from the surface of the transferred graphite alkyne for Raman spectrum characterization, the result shows that the graphite alkyne transferred to the target substrate is a continuous film and is relatively uniform, and the quality of the material cannot be damaged in the transfer process. The method solves the problem that large-area directional transfer of graphdyne grown on the copper foil by Glaser alkyne coupling reaction is difficult.
Drawings
FIG. 1 is a 200 Xlight mirror image of graphdine on the surface of a copper foil after etching by oxygen plasma reaction.
Fig. 2a and 2b are a 200 x optical and electron micrograph, respectively, of graphdyne transferred onto a target base silicon wafer.
Fig. 3a and 3b are 1000 x optical and electron micrographs, respectively, of a thin film of graphyne transferred onto a target substrate mark.
Fig. 4 is a raman spectrum of the graphite alkyne film after transfer.
Fig. 5a and 5b are AFM profiles of graphite alkyne films after transfer.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered in isolation, and they may be combined with each other to achieve better technical effects. In the drawings of the embodiments described below, the same reference numerals appearing in the various drawings denote the same features or components, and may be applied to different embodiments.
The invention adopts the following technical scheme:
a method for transferring large-area graphite alkyne film is characterized by that the graphite alkyne film on the copper foil which is undergone the process of oxygen plasma reaction etching and thinning is uniformly coated with polymethyl methacrylate, then placed in saturated ferric chloride solution to make reaction etching so as to obtain the invented copper foil. Firstly, fishing out the graphite alkyne film attached with polymethyl methacrylate from ferric chloride solution by using a silicon wafer, cleaning the graphite alkyne film in deionized water, fishing out the film by using a target substrate, drying the film for a certain time at a low temperature, then placing the film on a hot plate, heating the film for a certain time at a high temperature, and finally removing glue.
The method specifically comprises the following steps:
s1, uniformly coating polymethyl methacrylate on the graphite alkyne film on the copper foil which is thinned by the oxygen plasma reaction etching, and placing the graphite alkyne film in a saturated ferric chloride solution for reaction etching of the copper foil;
s2, fishing out the graphite alkyne film attached with polymethyl methacrylate from ferric chloride solution by using a clean silicon wafer, cleaning in deionized water, and fishing out the film by using a target substrate;
s3, heating by a hot plate for 40-60 ℃/5-7 min, heating for 180-250 ℃/3-6 min to enable the graphite alkyne film to be tightly attached to a target substrate, finally placing in an acetone solution for heating for 85-95 ℃/10-15 min to remove glue, taking out the graphite alkyne film from the acetone solution by using tweezers, quickly placing in an isopropanol solution for cleaning, taking out, and drying by nitrogen. Under an optical microscope, the graphite alkyne film with the size similar to that of the copper foil can be successfully transferred to the surface of the target substrate.
Furthermore, the graphyne is a film with the thickness of about 1 mu m, which is synthesized on the copper foil by taking hexaethynylbenzene as a monomer through Glaser alkyne coupling reaction, and the target substrate is SiO on the surface2U.S. silicon wafers having a thickness of about 300 nm.
Further, step S1 is specifically: uniformly coating polymethyl methacrylate on the surface of the graphdine on the copper foil which is etched and thinned by oxygen plasma reaction, scraping the graphdine on the surface without glue by using a knife, and putting the copper foil on the surface of a saturated ferric chloride solution with the surface facing downwards for standing for 12 hours to ensure that the copper foil can be completely reacted.
Further, step S2 is specifically: firstly, fishing out the polymethyl methacrylate film attached with the graphite alkyne from the ferric chloride solution by using a clean silicon wafer, putting the film into deionized water for cleaning for 3-4 times, and finally fishing out the film by using a target substrate, and paying attention to the fact that one surface attached with the graphite alkyne is attached to the target substrate.
In step S3, low-temperature drying is carried out for a period of time to remove moisture, so that the phenomenon that the material is damaged by the forced escape of water vapor in the high-temperature heating process can be prevented, and holes appear in the film graphite alkyne; the polymethyl methacrylate film with the graphite alkyne attached is easy to roll up and cannot be transferred continuously when the drying time is too long, and bubbles can be generated when the drying time is too short. Then heating at high temperature, wherein the graphite alkyne film can be tightly combined with the target substrate at the temperature of 180-250 ℃, so that the graphite alkyne attached to the polymethyl methacrylate can be completely transferred to the target substrate; and if the heating time is too long, the polymethyl methacrylate is difficult to completely remove subsequently, if the heating time is too short, the complete transfer of the graphite alkyne film cannot be realized, and multiple tests determine that the proper heating time range is 3-5 min, so that the large-area directional transfer of the graphite alkyne film can be realized.
Example 1
1. Uniformly coating polymethyl methacrylate on a graphite alkyne film (shown in figure 1) obtained by Glaser coupling reaction on the copper foil which is subjected to oxygen plasma reaction etching thinning, uniformly coating twice, heating at the temperature of 120 ℃/1min each time, and then placing the graphite alkyne film in a saturated ferric chloride solution for 12h to react and etch the copper foil;
2. taking a silicon wafer with an oxide layer with the thickness of 300nm and the size of 0.5cm multiplied by 0.5cm as a target substrate, fishing out the graphite alkyne film attached with polymethyl methacrylate from ferric chloride solution by using a clean silicon wafer, cleaning the silicon wafer in deionized water for 3-4 times, fishing out the film by using the target substrate, and paying attention to that one surface attached with graphite alkyne is in direct contact with the surface of the target substrate and spreading the surface of the target substrate flatly;
3. heating the graphite alkyne film on a hot plate at a speed of 50 ℃/5min for drying, then heating the graphite alkyne film at a speed of 250 ℃/5min for tightly adhering the graphite alkyne film to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating at a speed of 90 ℃/15min for removing glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the acetone alkyne film in an isopropanol solution for cleaning, fishing out the acetone alkyne film, and drying the acetone alkyne film by using nitrogen.
As shown in fig. 4, the graphite alkyne film with a size similar to that of the copper foil can be successfully transferred to the surface of the target substrate under an optical microscope, as shown in fig. 2a and fig. 2b, the optical microscope photograph and the electron microscope photograph are respectively 200 x optical microscope photograph and electron microscope photograph of the graphite alkyne film transferred to the silicon wafer, and the raman spectrum shows that the film quality is good.
Example 2
The embodiment of the invention provides a method for transferring a graphite alkyne film in a large area, which comprises the following steps:
1. uniformly coating polymethyl methacrylate on a graphite alkyne film obtained by Glaser coupling reaction on the copper foil which is subjected to the oxygen plasma reaction etching thinning, uniformly coating the polymethyl methacrylate twice, heating the graphite alkyne film at a temperature of 120 ℃/1min each time, and then placing the graphite alkyne film in a saturated ferric chloride solution for 12h to react and etch the copper foil;
2. mark with 400 field electrode pattern was used as the target substrate. The preparation process of the mark comprises the following steps: an inlet silicon wafer with an oxide layer with the thickness of 300nm → uniform photoresist, prebaking → ultraviolet exposure → postbaking, developing → thermal evaporation of metal Cr, Au → acetone solution for cleaning and removing the photoresist. Taking the obtained mark with the size of 0.5cm multiplied by 0.5cm as a target substrate, fishing out the graphite alkyne film attached with polymethyl methacrylate from a ferric chloride solution by using a clean silicon wafer, cleaning the graphite alkyne film in deionized water for 3-4 times, fishing out the film by using the target substrate, and paying attention to that one surface attached with graphite alkyne is directly contacted with the surface of the target substrate and flatly spreading the graphite alkyne;
3. heating the graphite alkyne film by a hot plate at 50 ℃/5min for drying, then heating the graphite alkyne film at 250 ℃/5min for tightly adhering the graphite alkyne film to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating at 90 ℃/15min for removing glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the graphite alkyne film in an isopropanol solution for cleaning, fishing out the graphite alkyne film, and drying the graphite alkyne film by using nitrogen. Under an optical microscope, the graphite alkyne film with the size similar to that of the copper foil is successfully transferred to the surface of the target substrate, as shown in a 1000 Xoptical microscope photo of the graphite alkyne film transferred to the mark of the target substrate in fig. 3a and an electron microscope photo of the graphite alkyne film transferred to the mark in fig. 3b, AFM analysis shows that the average thickness of the film is 15nm (as shown in fig. 5a and 5 b).
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above-mentioned serial numbers of the embodiments of the present invention are only for description, and do not represent the advantages and disadvantages of the embodiments.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The method for transferring the graphdiyne film in a large area is characterized by comprising the following steps of:
s1, uniformly coating polymethyl methacrylate on the graphite alkyne film on the copper foil which is subjected to the oxygen plasma reaction and etching thinning, and placing the graphite alkyne film in a saturated ferric chloride solution for reaction and etching, wherein the graphite alkyne film is a film which is synthesized on the copper foil by taking hexaethynylbenzene as a monomer through Glaser alkyne coupling reaction;
s2, fishing out the graphite alkyne film attached with polymethyl methacrylate from the saturated ferric chloride solution by using a clean silicon wafer, cleaning in deionized water, and fishing out the graphite alkyne film again by using a target substrate;
s3, heating and drying by a hot plate, then continuously heating to enable the graphite alkyne film to be tightly attached to a target substrate, finally placing the graphite alkyne film into an acetone solution to be heated and remove glue, fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the graphite alkyne film into an isopropanol solution to be cleaned, fishing out the graphite alkyne film, drying the graphite alkyne film by using nitrogen,
wherein, step S3 specifically includes: heating the graphite alkyne film by a hot plate for 40-60 ℃/5-7 min, then heating the graphite alkyne film for 180-250 ℃/3-6 min to enable the graphite alkyne film to be tightly attached to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating for 85-95 ℃/10-15 min to remove glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the acetone alkyne film in an isopropanol solution for cleaning, and then fishing out the graphite alkyne film and drying the graphite alkyne film by using nitrogen.
2. The method of claim 1, wherein the graphdine film has a thickness of 800 to 1000 nm.
3. The method of claim 1, wherein in step S2, the target substrate is surface SiO2A 300nm thick U.S. silicon wafer.
4. The method according to claim 1, wherein step S1 is specifically: uniformly coating polymethyl methacrylate on the surface of the graphite alkyne film on the copper foil subjected to the oxygen plasma reaction etching thinning, scraping off clean graphite alkyne from the surface of the graphite alkyne film which is not coated, placing the copper foil on the surface of a saturated ferric chloride solution with the surface facing downwards, standing for 12 hours for reaction etching, and completely reacting the copper foil.
5. The method according to claim 1, wherein step S2 is specifically: and fishing out the graphite alkyne film attached with the polymethyl methacrylate from the saturated ferric chloride solution by using a clean silicon wafer, putting the graphite alkyne film into deionized water for cleaning for 3-4 times, and finally fishing out the graphite alkyne film with the target substrate.
6. The method of claim 5, wherein in step S2, the side to which the thin film of graphdine is attached to a target substrate.
7. The method according to claim 1, wherein step S3 is specifically: heating the graphite alkyne film by a hot plate at 50 ℃/5min for drying, then heating the graphite alkyne film at 250 ℃/5min for tightly adhering the graphite alkyne film to a target substrate, finally placing the graphite alkyne film in an acetone solution for heating at 90 ℃/15min for removing glue, then fishing out the graphite alkyne film from the acetone solution by using tweezers, quickly placing the graphite alkyne film in an isopropanol solution for cleaning, fishing out the graphite alkyne film, and drying the graphite alkyne film by using nitrogen.
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| CN108793100A (en) * | 2018-06-30 | 2018-11-13 | 中国人民解放军国防科技大学 | Atomic-level thickness graphene/boron nitride composite heterogeneous film transfer method |
| CN110668436A (en) * | 2019-11-04 | 2020-01-10 | 北京科技大学 | Preparation method of ultrathin nanoscale graphite alkyne film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201704950D0 (en) * | 2017-03-28 | 2017-05-10 | Univ Manchester | Thin film material transfer method |
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| CN102351175A (en) * | 2011-11-03 | 2012-02-15 | 东南大学 | High-quality transfer method of graphene prepared by chemical vapor deposition method |
| CN102897759A (en) * | 2012-10-17 | 2013-01-30 | 东南大学 | Loss-less transfer method for large-size graphene |
| CN107585762A (en) * | 2017-08-11 | 2018-01-16 | 江苏大学 | A kind of modification method of copper foil substrate graphene transfer |
| CN107867683A (en) * | 2017-10-20 | 2018-04-03 | 上海健康医学院 | A kind of transfer method of large-area high-quality graphene |
| CN108793100A (en) * | 2018-06-30 | 2018-11-13 | 中国人民解放军国防科技大学 | Atomic-level thickness graphene/boron nitride composite heterogeneous film transfer method |
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