CN111320164A - Preparation method of suspended graphene structure, suspended graphene structure obtained by preparation method and application of suspended graphene structure - Google Patents
Preparation method of suspended graphene structure, suspended graphene structure obtained by preparation method and application of suspended graphene structure Download PDFInfo
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- CN111320164A CN111320164A CN202010127240.3A CN202010127240A CN111320164A CN 111320164 A CN111320164 A CN 111320164A CN 202010127240 A CN202010127240 A CN 202010127240A CN 111320164 A CN111320164 A CN 111320164A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 72
- 239000010410 layer Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 238000010894 electron beam technology Methods 0.000 claims abstract description 18
- 238000000059 patterning Methods 0.000 claims abstract description 11
- 239000012790 adhesive layer Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000000693 micelle Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 238000004528 spin coating Methods 0.000 claims description 7
- 239000002390 adhesive tape Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- 239000000463 material Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000003292 glue Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 238000005530 etching Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000007481 next generation sequencing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000003825 pressing 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
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 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
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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Abstract
The invention provides a preparation method of a suspended graphene structure, the suspended graphene structure obtained by the preparation method and application of the suspended graphene structure, wherein the preparation method comprises the following steps: (1) patterning the membrane to be processed to obtain a patterned area and other areas; the membrane to be processed comprises a sacrificial layer, a graphene sheet layer and an electron beam adhesive layer which are sequentially arranged; the patterning process comprises exposing a partial region of the graphene sheet; (2) and sequentially removing the rest regions and the sacrificial layer, and then transferring the patterned region to the substrate to obtain the suspended graphene structure. The preparation method provided by the invention does not relate to corrosive liquid, is simple in operation process, and is easy to transfer and assemble graphene. The preparation method provided by the invention can realize the preparation of suspended structures of graphene materials with different shapes and sizes, and can also be used for any substrate.
Description
Technical Field
The invention belongs to the field of graphene preparation, and relates to a preparation method of a suspended graphene structure, the suspended graphene structure obtained by the preparation method and application of the suspended graphene structure.
Background
Graphene is a two-dimensional film composed of carbon atoms and having a honeycomb structure. Due to excellent electron mobility, thickness of a monoatomic layer and ultrahigh mechanical strength, the material is considered to have wide application prospects in a plurality of fields such as information technology, semiconductors, biosensing, energy and environmental protection.
In the field of semiconductor technology, graphene is considered to be a possible base material for next-generation semiconductor technology instead of silicon due to its excellent electrical properties. Conventional graphene is typically grown on or transferred onto an insulating substrate and then used to fabricate functional devices. However, the interaction of graphene with the substrate may reduce the electron mobility of graphene, thereby reducing the performance of the graphene functional device. In addition, the graphene has wide application prospect in the field of molecular detection, and the preparation of high-quality suspended graphene is a key step of the method. For example, graphene-based nanopores are considered to have potential applications in the field of biosensing, particularly next generation DNA sequencing technologies. Therefore, the preparation of suspended graphene has been one of the efforts of technicians in related fields.
CN109824046A discloses a method for preparing a suspended graphene support film of Janus structure, which comprises: growing a graphene film on the surface of a metal substrate by a chemical vapor deposition method, preparing a suspended graphene film, finally placing the obtained suspended graphene in a plasma cleaning machine, and carrying out functional treatment on the surface of the graphene to obtain the Janus graphene support film with controllable hydrophilicity and hydrophobicity and high integrity (80%). At present, the preparation of suspended graphene is mainly a transfer method or an etching method. The former is to transfer the prepared graphene to a substrate with a structure to form a suspended functional region; and etching the substrate below the graphene to obtain the suspended graphene. The etching method usually uses corrosive liquid, the preparation process is complicated, the control difficulty is high, and the potential performance of the suspended graphene can be influenced by inevitable chemical pollution.
CN104787754A discloses a preparation method of suspended graphene, which comprises the following steps: step A, preparing an expected structure on a silicon carbide substrate by adopting a semiconductor process, and step B, preparing suspended graphene by adopting a high-temperature decomposition method in a carbon-rich environment. Although the patent application does not apply an etching technology, the prepared suspended graphene cannot be transferred and applied.
Therefore, it is desirable to provide a preparation method of a suspended graphene structure, which is simple to operate, so as to meet application requirements.
Disclosure of Invention
The invention aims to provide a preparation method of a suspended graphene structure, the suspended graphene structure obtained by the preparation method and application of the suspended graphene structure. The preparation method provided by the invention does not relate to corrosive liquid, is simple in operation process, and is easy to transfer and assemble graphene. The preparation method provided by the invention can realize the preparation of suspended structures of graphene materials with different shapes and sizes, and can also be used for any substrate.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a suspended graphene structure, the method comprising the following steps:
(1) patterning the membrane to be processed to obtain a patterned area and other areas;
the membrane to be processed comprises a sacrificial layer, a graphene sheet layer and an electron beam adhesive layer which are sequentially arranged;
the patterning process comprises exposing a partial region of the graphene sheet;
(2) and sequentially removing the rest regions and the sacrificial layer, and then transferring the patterned region to the substrate to obtain the suspended graphene structure.
The preparation method provided by the invention is simple to operate, and can realize the exposure of the graphene sheet by using electron beam glue exposure, thereby realizing the subsequent preparation of the graphene suspended structure.
Preferably, the preparation method of the membrane to be treated comprises the following steps:
preparing a sacrificial layer on a substrate by using spin coating, arranging a single-layer graphene sheet on the sacrificial layer by using an adhesive tape, and arranging an electronic micelle layer on the graphene sheet layer by using spin coating to obtain the membrane to be processed.
Preferably, the sacrificial layer is selected from a polyvinyl alcohol layer.
Preferably, the electron micelle layer is selected from a polymethylmethacrylate layer.
According to the invention, polyvinyl alcohol is selected as the sacrificial layer, and the polyvinyl alcohol is dissolved in water, so that the sacrificial layer is easy to remove, and meanwhile, the existence of the sacrificial layer does not generate any adverse effect on the graphene sheet and the patterning treatment. According to the invention, through the cooperation of the sacrificial layer and the electronic micelle layer, part of the area of the graphene sheet can be exposed and is not adhered to other materials, which is a necessary requirement for forming a graphene suspended structure in the later stage.
Preferably, the patterning process is performed by electron beam exposure.
The invention adopts a flexible electron beam exposure process, can realize the preparation and the transfer of the graphene suspended structures with different shapes and sizes, and particularly does not need to process the substrate, so the substrate after the transfer does not need to be considered, and the invention can be suitable for any substrate.
Preferably, there is at least one connection between the patterned region and the remaining region.
Preferably, the width of the connection is 1-2 μm, such as 1.2 μm, 1.5 μm, 1.8 μm, etc.
Preferably, an opening region is further disposed in the patterned region.
Preferably, the diameter of the open region is 2-3 μm, such as 2.2 μm, 2.5 μm, 2.8 μm, and the like.
The patterned region obtained by patterning treatment is weakly connected with other parts (only connected by a plurality of connecting parts with extremely small widths), so that the patterned region can be easily transferred by only utilizing a microneedle (the tip is less than 1-2 mu m) through an open hole region designed in the patterned region in the subsequent treatment process; and the graphene exposed area is a sample window in the subsequent application process.
Because partial areas of the graphene sheets are exposed, namely the periphery of each graphene sheet is provided with the electron beam glue, after the graphene sheets are transferred to the substrate, the electron beam glue and the substrate have better cohesiveness compared with the graphene sheets, so that the electron beam glue at the periphery of each graphene sheet is attached to the substrate, the graphene sheets are in a bulging state, and suspension of the graphene sheets is realized.
Preferably, the method for removing the sacrificial layer is a water immersion method.
Preferably, the water immersion method is to immerse the membrane to be treated in water to remove the sacrificial layer.
Preferably, the temperature of the water is 50-100 ℃, such as 60 ℃, 70 ℃, 80 ℃, 90 ℃ and the like.
Preferably, the method for removing the remaining region in the step (2) is: microscopically, the microneedle is used to penetrate the open area, pick out the patterned area, and remove the rest of the area.
Preferably, the substrate is selected from silicon wafers.
In a second aspect, the invention provides a suspended graphene structure prepared by the preparation method according to the first aspect.
In a third aspect, the invention provides a use of the suspended graphene structure according to the second aspect in the preparation of a micro-electromechanical system (MEMS).
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method provided by the invention is simple to operate, and can realize the exposure of the graphene sheet by using electron beam glue exposure, thereby realizing the preparation of the subsequent graphene suspended structure;
(2) according to the invention, polyvinyl alcohol is selected as the sacrificial layer, and the polyvinyl alcohol is dissolved in water, so that the sacrificial layer is easy to remove, and meanwhile, the existence of the sacrificial layer does not generate any adverse effect on the graphene sheet and the patterning treatment. According to the invention, through the cooperation of the sacrificial layer and the electronic micelle layer, part of the area of the graphene sheet can be exposed and is not adhered to other materials, which is a necessary requirement for forming a graphene suspended structure in the later stage;
(3) the invention adopts a flexible electron beam exposure process, can realize the preparation and the transfer of the graphene suspended structures with different shapes and sizes, and particularly does not need to process the substrate, so the substrate after the transfer does not need to be considered, and the invention can be suitable for any substrate.
Drawings
Fig. 1 is a schematic structural diagram of a membrane to be processed according to embodiment 1 of the present invention.
Fig. 2 is a schematic structural view of the structure after the sacrificial layer is removed in embodiment 1 of the present invention.
Wherein, 1-a substrate; 2-a sacrificial layer; 3-an electron micelle layer; 301-a connecting portion; 302-an open area; 4-graphene lamellae; 401-graphene sheets.
Fig. 3 is a high tilt angle scanning electron microscope photograph of the graphene suspended structure provided in embodiment 1.
Fig. 4 is a high tilt angle scanning electron microscope photograph of unsettled graphene attached to an electrode.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
A preparation method of a suspended graphene structure comprises the following steps:
(1) as shown in fig. 1, a to-be-treated membrane is prepared by spin coating of a spin coater and stripping of an adhesive tape;
the membrane to be processed is composed of a substrate 1, a sacrificial layer 2, a graphene sheet layer 4 and an electron beam glue layer 3 which are sequentially arranged.
Firstly, dripping a PVA aqueous solution (the solid content is 4%) on a silicon wafer, spin-coating by a spin coater, and baking by a hot table to obtain a sacrificial layer. And peeling off the natural graphite by using an adhesive tape, covering the surface of the sacrificial layer with the adhesive tape with the graphite sheets, slightly applying pressure by using hands, and removing the adhesive tape to ensure that partial graphite sheets are remained on the sacrificial layer. Dropping an electron beam glue solution (6 mass percent of PMMA (methyl methacrylate) with the molecular weight of 950K) on the sacrificial layer with the graphite sheet, spin-coating by a spin coater, and drying by a hot table to obtain the membrane to be processed.
(2) Carrying out patterning treatment on the membrane to be treated by utilizing electron beam exposure to obtain a patterned area and other areas;
wherein the parameters of the electron beam are 30KV and the exposure dose is 1000 uC/cm2;
As shown in fig. 2, 6 connecting parts 301 are arranged between the patterned region and the rest regions, the width of each connecting part 301 is 1 μm, the patterned region comprises a part of the region, which is exposed to the graphene sheet 401, and is further provided with an opening region 302, and the diameter of the opening region 302 is 3 μm;
(3) soaking the membrane to be treated processed in the step (2) in water at 80 ℃, removing the sacrificial layer, and fishing out the rest parts (the electron beam glue layer and the graphene sheet layer) by using metal wires;
(4) and (3) adopting a microneedle drawn by a glass tube, picking out a patterned area from the electron beam adhesive layer by using a hydraulic displacement operating platform under an optical microscope, aligning the patterned area with a target substrate, and covering the target substrate to obtain the graphene suspended structure.
Structural characterization
The graphene suspended structure prepared in example 1 was observed by a scanning electron microscope, and the results were as follows:
fig. 3 is a high tilt angle scanning electron microscope photograph of the graphene suspension structure provided in embodiment 1, and fig. 4 is a high tilt angle scanning electron microscope photograph of non-suspended graphene attached to an electrode; as can be seen from a comparison between fig. 3 and fig. 4, in fig. 3, the graphene has an inclined angle, and there is a significant gap between the graphene and the substrate electrode, so that the suspended graphene structure is obtained by the present invention.
The applicant states that the present invention uses the above embodiments to illustrate the preparation method of the suspended graphene structure of the present invention, and the suspended graphene structure obtained therefrom and applications, but the present invention is not limited to the above process steps, i.e. it does not mean that the present invention must rely on the above process steps to be implemented. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.
Claims (10)
1. A preparation method of a suspended graphene structure is characterized by comprising the following steps:
(1) patterning the membrane to be processed to obtain a patterned area and other areas;
the membrane to be processed comprises a sacrificial layer, a graphene sheet layer and an electron beam adhesive layer which are sequentially arranged;
the patterning process comprises exposing a partial region of the graphene sheet;
(2) and sequentially removing the rest regions and the sacrificial layer, and then transferring the patterned region to the substrate to obtain the suspended graphene structure.
2. The method for preparing a membrane according to claim 1, wherein the method for preparing a membrane to be treated comprises the following steps:
preparing a sacrificial layer on a substrate by using spin coating, arranging a single-layer graphene sheet on the sacrificial layer by using an adhesive tape, and arranging an electronic micelle layer on the graphene sheet layer by using spin coating to obtain the membrane to be processed.
3. The production method according to claim 1 or 2, characterized in that the sacrificial layer is selected from a polyvinyl alcohol layer;
preferably, the electron micelle layer is selected from a polymethylmethacrylate layer.
4. The production method according to any one of claims 1 to 3, wherein the pattern processing is performed by electron beam exposure.
5. A method of manufacturing according to any of claims 1-4, wherein there is at least one connection between the patterned region and the remaining region;
preferably, the width of the connecting part is 1-2 μm;
preferably, an opening region is further arranged in the patterned region;
preferably, the diameter of the open region is 2-3 μm.
6. The production method according to any one of claims 1 to 5, wherein the method of removing the sacrifice layer is a water immersion method;
preferably, the water immersion method is to immerse the membrane to be treated in water and remove the sacrificial layer;
preferably, the temperature of the water is 50-100 ℃.
7. The production method according to any one of claims 1 to 6, wherein the remaining region of step (2) is removed by: microscopically, the microneedle is used to penetrate the open area, pick out the patterned area, and remove the rest of the area.
8. The production method according to any one of claims 1 to 7, wherein the substrate is selected from a silicon wafer.
9. The suspended graphene structure prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the suspended graphene structure of claim 9 in the preparation of a microelectromechanical system.
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JPS55105331A (en) * | 1979-02-08 | 1980-08-12 | Nec Corp | Method for forming electronic-beam resist pattern on electrical insulating material |
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CN104217928A (en) * | 2013-05-30 | 2014-12-17 | 清华大学 | Fabrication method of nano-scale micro structure |
CN109824046A (en) * | 2019-03-27 | 2019-05-31 | 北京大学 | A method of preparing the hanging graphene support membrane of Janus structure |
-
2020
- 2020-02-28 CN CN202010127240.3A patent/CN111320164A/en active Pending
Patent Citations (6)
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