CN113548642A - Preparation method of graphene nano electrode pair array with continuous and controllable gaps on chip - Google Patents
Preparation method of graphene nano electrode pair array with continuous and controllable gaps on chip Download PDFInfo
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- CN113548642A CN113548642A CN202110822784.6A CN202110822784A CN113548642A CN 113548642 A CN113548642 A CN 113548642A CN 202110822784 A CN202110822784 A CN 202110822784A CN 113548642 A CN113548642 A CN 113548642A
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- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B82—NANOTECHNOLOGY
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Abstract
A preparation method of a graphene nano electrode pair array with continuous and controllable gaps on a chip relates to a graphene chip which is composed of a piezoelectric piece, polyimide and a graphene electrode, wherein the piezoelectric piece and the polyimide are used as substrates, the graphene electrode is fixed above the polyimide through adsorption force, the graphene electrode transfers an electrode pattern to graphene/PMMA through a hollowed mask and a coating processing technology, and the graphene is etched into an electrode shape by utilizing a reactive ion etching technology; the graphene electrode is stretched by regulating and controlling the voltage applied to the piezoelectric sheet to expand and extend along the horizontal direction, the graphene electrode is blown to form a gap by an electromigration method, and the distance between the electrodes is precisely adjusted by the expansion and contraction of the piezoelectric sheet. The method has simple process and low cost, realizes the on-chip large-scale integration of the graphene electrode with controllable gap, and lays a foundation for the development of carbon-based molecular electronic devices.
Description
Technical Field
The invention belongs to a preparation method of an on-chip continuous gap-controllable graphene nano electrode pair array, and relates to the fields of molecular electronics, nano materials, chemistry and the like.
Background
In the trend of miniaturization of electronic devices, molecular electronics has been rapidly developed in recent years. Molecular electronics constructs molecular junctions, and the logical functions of the traditional devices are realized through regulation and control by various means. Moreover, compared with the multi-molecule junction, the single-molecule junction is developed more greatly.
The unimolecular junction is formed by embedding a single molecule between two nano electrodes, namely an electrode-unimolecular-electrode junction, and the key for constructing the unimolecular junction is to match the gap between the electrodes with the length of the molecule and ensure that the molecule is stably connected with the electrodes at two ends. In general, the electrodes of the single-molecule junctions are mainly made of noble metals such as gold, platinum, and silver, and form metal-single-molecule-metal junctions. But the metal electrode is easy to be oxidized under the experimental environment condition and forms non-ohmic contact with molecules; and the electron state density distribution near the fermi level is relatively narrow, so that the construction of a molecular junction is difficult. Compared with the graphene, the graphene has the advantages of low cost, high mechanical strength, wide electronic state density distribution at the Fermi level and the like, and more importantly, the graphene electrode can be connected with molecules through covalent bonds, so that the molecular structure is easier to construct, and the performance of the formed molecular device is more stable.
To date, there are many techniques for constructing graphene monomolecular junctions by constructing graphene electrodes having sub-nanometer gaps, and the most representative techniques include: electromigration, scanning probe microscopy, mechanically controlled fracture junction, and the like. And the respective realization processes are combined with micro-nano processing technology. However, each of these technologies has its advantages and disadvantages, which mainly focus on the following points:
1. the distance of the gaps of the sub-nanometer gap electrodes which can be integrated on the chip cannot be continuously and repeatedly adjusted after the sub-nanometer gap electrodes are constructed, so that the success rate of forming the gaps matched with the lengths of molecules is low;
2. the electrode capable of regulating and controlling the gap needs a fine displacement device for regulation and control in the process of constructing a molecular junction test, is sensitive to external vibration and has high cost;
3. in the process of constructing the gap-adjustable molecular junction, the molecular junction is displaced in the direction vertical to the chip, so that the integration on the chip is impossible, and the large-scale integration of the graphene molecular junction as an electronic circuit component is limited.
The prior art document 2017103609180 introduces a method for preparing a single-layer graphene monomolecular junction with a mechanically controllable nanogap, which cannot perform on-chip integration and realize a high-yield stable molecular junction, and adopts piezoelectric ceramics with high cost to finely regulate and control a graphene electrode gap.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a method for preparing an on-chip graphene nano electrode pair array with continuously controllable gaps. The single molecule is efficiently connected by accurately controlling the distance between electrodes, so that the carbon-based single molecule electronic component is prepared on a high-yield large-area ground, and an effective method is provided for the integration of molecular electronic components.
The purpose of the invention is realized as follows:
a preparation method of a graphene nano electrode pair array with continuous and controllable gaps on a chip comprises a piezoelectric sheet, polyimide and a graphene electrode, wherein the piezoelectric sheet and the polyimide are used as substrates, and the graphene electrode is formed by processing graphene into an electrode shape and fixing the electrode shape above the polyimide through adsorption force; and continuously controllable voltage is applied to the piezoelectric sheet to enable the piezoelectric sheet to expand and extend, and meanwhile, the graphene electrode is blown by an electromigration method to form a tiny gap.
Furthermore, the expansion and contraction quantity of the piezoelectric sheet is controlled by applying continuously controllable voltage on the piezoelectric sheet, so that the accurate continuous control of the gap size of the graphene electrode integrated on the sheet is realized, and the expansion and contraction directions of the piezoelectric sheet are horizontal; the polyimide insulating layer is used for isolating the piezoelectric sheet from the graphene and flattening the surface of the piezoelectric sheet.
Further, large-area single-layer or few-layer graphene grown by a Chemical Vapor Deposition (CVD) method is used as an electrode material; the surface of graphene is coated with a layer of polymethyl methacrylate (PMMA) firstly, and then copper foil is placed in FeCl3And (3) corroding the copper foil in the solution, and transferring the graphene/PMMA onto a piezoelectric sheet coated with polyimide.
Further, the on-chip graphene micro-nano electrode is constructed, an electrode pattern is transferred to PMMA through a hollow coating mask and a coating processing technology, graphene is etched into an electrode shape through a reactive ion etching technology, and finally the PMMA and a metal layer on the PMMA are removed through acetone, so that the large-scale graphene electrode array is prepared.
Furthermore, the voltage applied to the piezoelectric sheet is regulated and controlled to enable the piezoelectric sheet to expand and extend along the horizontal direction, so that the graphene electrode is stretched, the graphene electrode is blown to form a gap by an electromigration method, and a tiny groove is formed in the middle of the insulating layer polyimide in the process of etching the reaction ion beam and expanding and extending the piezoelectric sheet along the horizontal direction, so that the fracture part of the graphene electrode is suspended, the electrode pair can freely move along with the expansion and contraction of the piezoelectric sheet, and the distance between the electrodes can be precisely adjusted.
Further, the piezoelectric sheet and the polyimide as the substrate are obtained by: and diluting the insulating glue polyimide and the N-methylpyrrolidone according to the mass ratio of 5:1, and spin-coating the diluted insulating glue on the cleaned piezoelectric sheet by a spin coater twice. The two-time spin coating method comprises the steps of adopting 2000rpm for the first spin coating, adopting 3500rpm for the second spin coating, placing the first spin coating on a heating table at 70 ℃ for baking for half an hour, and placing the second spin coating on a heating table at 80 ℃ for baking for 2 hours.
The invention has the advantages that:
the method comprises the steps of transferring graphene to the surface of a piezoelectric plate coated with a polyimide insulating layer by using a PMMA method, preparing a graphene electrode array by using a hollow mask through a series of processes such as film coating and ion beam etching, breaking electrodes by using an electromigration method to form an electrode pair, and realizing accurate continuous controllability of a nanometer gap by using expansion and contraction of piezoelectricity. The method has simple and easy process and low cost, can control the gap of the electrodes on a plane, and is convenient for large-area integration on a chip; because the suspended part of the fracture part is extremely few, and the electrodes are integrated on the same substrate and are not easily influenced by external vibration, the displacement precision of the regulation and control molecular gap is extremely high, the problem that the electrode gap prepared by an electromigration method cannot be changed is further solved, molecules can be efficiently connected to the two ends of the electrodes, and finally the single-layer graphene monomolecular junction manufactured in high yield is realized; compared with a metal monomolecular junction, the graphene all-carbon electronic junction has better stability and conductivity, and the circuit can be directly connected to two ends of the graphene electrode by adopting the all-graphene electrode without secondary alignment, so that a good foundation is laid for an all-carbon electronic circuit.
Drawings
In order to make the object and technical solution of the present invention more clear, the present invention will be further described in detail with reference to the attached drawings of a single electrode in an array electrode:
FIG. 1 shows a piezoelectric sheet 1 coated with polyimide 2 as an insulating layer;
FIG. 2 is a schematic diagram of a Chemical Vapor Deposition (CVD) method based on FIG. 1, in which large-area single-layer or multi-layer graphene 3 grown on a copper foil is coated with a layer of polymethyl methacrylate (PMMA)4 on the surface of the graphene, and then the copper foil is placed in FeCl3The method for corroding the copper foil in the solution comprises the steps of transferring graphene to a piezoelectric sheet 1 coated with polyimide;
FIG. 3 is a view showing that the hollowed-out metal mask 5 is tightly pressed on the PMMA4 based on FIG. 2;
fig. 4 is a general view of the top view of the electrode array of the metal mask 5 shown in fig. 3, wherein the hollow portion is hollow;
FIG. 5 is a schematic view of the process of FIG. 3, in which a metal layer 6 is deposited on PMMA4 by Physical Vapor Deposition (PVD) to form a hollow-out portion of a metal mask 5;
fig. 6 is a diagram illustrating that, on the basis of fig. 5, the polyimide 2, the graphene 3 and the PMMA4 on the piezoelectric sheet 1 are etched into a shape like the metal layer 6 by a reactive ion etching technique using the metal layer 6 as a protective layer;
FIG. 7 is based on FIG. 6, in which the PMMA4 on the electrode is removed by acetone, and the metal layer 6 on the electrode is removed;
fig. 8 is based on fig. 7, the graphene electrode is stretched in the X direction by adjusting and controlling the voltage applied to the piezoelectric sheet to expand and elongate in the horizontal direction, and the graphene 3 is blown by the electromigration method to form the gap 7. In the process of reactive ion beam etching and expansion and elongation of the piezoelectric sheet along the horizontal direction, the polyimide 2 below the graphene electrode pair is used as an insulating layer, and a small groove is formed in the middle of the polyimide 2, so that the fracture part of the graphene electrode is suspended, the electrode pair can freely move along with expansion and contraction of the piezoelectric sheet, and the distance between the electrodes can be precisely adjusted.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Referring to the attached drawing 1, firstly, a layer of polyimide 2 is coated on a piezoelectric sheet 1 to serve as an insulating layer, and specifically, the piezoelectric sheet is ultrasonically cleaned for 5min by ethanol, isopropanol, acetone and ethanol according to the flow sequence, so that the surface pollutants are cleaned. Finally, the mixture is cleaned by purified water and dried by nitrogen with small flow. And taking a proper amount of insulating glue polyimide (HD-4100) and N-methyl pyrrolidone to dilute according to the mass ratio of 5: 1. And spin-coating the diluted insulating glue on the cleaned piezoelectric plate 1 by a spin coater twice. 2000rpm is adopted in the first spin coating, 3500rpm is adopted in the second spin coating, and the surface of the piezoelectric sheet 1 is ensured to have an insulation effect. After the first spin coating, the mixture is placed on a heating table at 70 ℃ and baked for half an hour to play a role in curing; after the second spin coating, the coating is baked for 2 hours at 80 ℃ so that the insulating glue can be amidated to achieve an insulating effect. Referring to FIG. 2, chemical vapor deposition will then be utilizedLarge-area single-layer or multi-layer graphene 3 grown on copper foil by an integral deposition (CVD) method is prepared by firstly coating a layer of polymethyl methacrylate (PMMA)4 on the surface of graphene, and then placing the copper foil in FeCl3The method for corroding the copper foil in the solution comprises the steps of transferring graphene to a piezoelectric sheet 1 coated with polyimide 2; referring to fig. 3, the hollowed-out metal mask 5 is tightly pressed on the PMMA 4; FIG. 4 is a top view of the electrode array of the metal mask 5, wherein the hollow part is hollow; referring to fig. 5, a metal layer 6 with a thickness of about 100nm is deposited on PMMA4 by a Physical Vapor Deposition (PVD) method, and the deposited shape is the same as the hollow part in the metal mask 5; referring to fig. 6, the polyimide 2, the graphene 3 and the PMMA4 on the piezoelectric sheet 1 are etched into a shape like the metal layer 6 by a reactive ion etching technique using the metal layer 6 as a protective layer; referring to fig. 7, the PMMA4 on the electrode is removed by acetone, and the metal layer 6 thereon is removed; referring to fig. 8, a continuously controllable voltage is applied to the piezoelectric sheet to expand and extend the piezoelectric sheet along the X direction, and at the same time, the graphene electrode 3 is blown by an electromigration method to form a minimum gap 7, and the polyimide 2 below the graphene electrode is used as an insulating layer to form a minimum suspension in the processes of reactive ion beam etching and expansion and extension of the piezoelectric sheet along the X direction, so that the electrode pair can freely move along with expansion and contraction of the piezoelectric sheet, thereby precisely adjusting the distance between the electrodes.
The invention relates to a preparation method of a graphene electrode pair array, which is based on a piezoelectric material and combines an electromigration method and a micro-nano processing technology to construct graphene into a large-scale controllable gap on a sheet, and can prepare a large amount of graphene monomolecular junctions with high success rate. The electromigration method specifically refers to an 'electrical burning' method with feedback regulation, namely, a voltage is applied to a graphene sheet layer subjected to micro-nano processing, when a current suddenly drops at a certain point, a monitoring system is fed back in real time and repeatedly scanned, the scanning is repeated, the operation is repeated, and a graphene nanoribbon is opened by using joule heat generated by the current to form a graphene electrode with a clean surface. The reciprocating expansion and contraction motion of the piezoelectric sheet is controlled, so that molecular junctions are formed and broken rapidly, massively and repeatedly; once the molecular junction is formed, the molecular junction can exist extremely stably, and the research on the electron transport characteristics of the molecular junction adjusted by means of other light, magnetism, gate voltage, pH and the like is facilitated, and the functional molecular electronic device is integrated in the later period.
The method has simple process, low cost and stable molecular junction, most importantly realizes large-scale on-chip integration of the continuous controllable gap electrode, and provides an effective method for preparing the graphene monomolecular junction with high success rate and constructing the carbon-based molecular electronic device; meanwhile, a foundation is laid for realizing a high-performance molecular device, and the method has a high reference value for the development of molecular electronics.
Claims (7)
1. A preparation method of an on-chip continuous gap-controllable graphene nano electrode pair array is characterized by comprising the following steps of: the piezoelectric film is composed of a piezoelectric sheet, polyimide and a graphene electrode;
the piezoelectric sheet and the polyimide are used as substrates, and the graphene electrode is formed by processing graphene into an electrode shape and fixing the electrode shape above the polyimide through adsorption force;
and continuously controllable voltage is applied to the piezoelectric sheet to enable the piezoelectric sheet to expand and extend, and meanwhile, the graphene electrode is blown by an electromigration method to form a tiny gap.
2. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 1, wherein the method comprises the following steps: the piezoelectric sheet and the polyimide are used as substrates to regulate and control the gap between the electrode pairs; the expansion and contraction amount of the controller is controlled by applying continuously controllable voltage on the piezoelectric sheet, so that the accurate continuous control of the gap size of the graphene electrode integrated on the sheet is realized, and the expansion and contraction directions of the piezoelectric sheet are horizontal; the polyimide insulating layer is used for isolating the piezoelectric and the graphene and flattening the surface of the piezoelectric sheet.
3. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 1, wherein the method comprises the following steps: large-area single-layer or few-layer graphene grown by Chemical Vapor Deposition (CVD) is used as an electrode material; by firstCoating a layer of polymethyl methacrylate (PMMA) on the surface of graphene, and then placing a copper foil in FeCl3And (3) corroding the copper foil in the solution, and transferring the graphene/PMMA onto a piezoelectric sheet coated with polyimide.
4. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 1, wherein the method comprises the following steps: the construction of the on-chip graphene micro-nano electrode is that firstly, an electrode pattern is transferred onto PMMA through a hollow coating mask and a coating processing technology, then graphene is etched into an electrode shape through a reactive ion etching technology, and finally, the PMMA and a metal layer on the PMMA are removed through acetone, so that a large-scale graphene electrode array is obtained.
5. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 4, wherein the method comprises the following steps: the utility model discloses a graphite alkene electrode is to the formation and regulation and control of clearance between the graphite alkene electrode pair, thereby earlier make its along the horizontal direction expansion extension stretch graphite alkene electrode tensile through regulating and controlling the voltage that applies on the piezoelectric patches, utilize the electromigration method to blow graphite alkene electrode simultaneously and form the clearance, at reaction ion beam etching and piezoelectric patches along the in-process of horizontal direction expansion extension, insulating layer polyimide mid portion produces a minimum recess, it is unsettled to realize graphite alkene electrode fracture department part, make the electrode pair can freely remove along with the expansion and the shrink of piezoelectric patches, thereby the distance between accurate regulation electrode.
6. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 1, wherein the method comprises the following steps: the piezoelectric sheet and polyimide as substrates were obtained by the following methods: and diluting the insulating glue polyimide and the N-methylpyrrolidone according to the mass ratio of 5:1, and spin-coating the diluted insulating glue on the cleaned piezoelectric sheet by a spin coater twice.
7. The method for preparing the graphene nano electrode pair array with the continuous controllable gap on the chip according to claim 6, wherein the method comprises the following steps: the two spin coating methods are that the first spin coating adopts 2000rpm, the second spin coating adopts 3500rpm, after the first spin coating, the first spin coating is placed on a heating table at 70 ℃ to be baked for half an hour, and after the second spin coating, the second spin coating is placed at 80 ℃ to be baked for 2 hours.
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| CN114709280A (en) * | 2022-03-28 | 2022-07-05 | 国家纳米科学中心 | Photoelectric detector and preparation method thereof |
| CN115636389A (en) * | 2022-10-14 | 2023-01-24 | 南开大学 | Preparation method and application of monomolecular junction based on controllable nanogap of piezoelectric sheet |
| CN115980131A (en) * | 2022-10-25 | 2023-04-18 | 南开大学 | Planar mechanical controllable junction cracking technology based on flexible material |
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