CN116075207A - Nondestructive preparation method of two-dimensional superconducting nano integrated circuit - Google Patents
Nondestructive preparation method of two-dimensional superconducting nano integrated circuit Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Abstract
The invention discloses a nondestructive preparation method of a two-dimensional superconducting nano integrated circuit, which is characterized by comprising the following steps of: firstly, growing an ultrathin transition metal film on a substrate; then, the nano integrated circuit device of the superconducting metal film is obtained by electron beam exposure and reactive ion etching; then, the metal film nano device is converted into a nano integrated device of a two-dimensional superconducting film in situ by using a topological chemical conversion method; and finally, growing a layer of insulating material on the device to obtain the two-dimensional superconducting nano integrated circuit. The invention effectively avoids the damage effect of the traditional micro-nano processing flow on the low-dimensional material, and realizes the nondestructive preparation of various low-dimensional material devices. Meanwhile, the scheme can be used for preparing various device structures, so that the performance of the device can be regulated and controlled.
Description
Technical Field
The invention belongs to the technical field of micro-nano processing and preparation of two-dimensional superconducting materials, and particularly relates to a nondestructive preparation method of a two-dimensional superconducting nano integrated circuit.
Background
In inorganic semiconductor films, when the film thickness is reduced to the limit of two-dimensional materials, the film tends to undergo a novel series of characteristic changes. For example, the conductivity of graphene can change along with the thickness; the low-dimensional perovskite material has higher carrier mobility and exciton binding energy and is widely applied to light-emitting elements such as detectors, LEDs and the like; the band gap of the transition metal chalcogenide compound increases with decreasing number of layers; likewise, when the thickness of the two-dimensional laminar superconducting film is reduced to a single layer or several layers, the superconducting electrical property and the optical property of the two-dimensional laminar superconducting film are more excellent and easy to regulate than those of a bulk material.
At present, growing transition metal chalcogenides mainly involves the following methods: mechanical exfoliation, lithium ion intercalation, liquid phase exfoliation, chemical vapor deposition. (1) mechanical stripping method. The method mainly comprises the steps of placing a crystal material with a two-dimensional structure to be stripped on a transparent adhesive tape, and then repeatedly pasting to obtain an ultrathin lamellar sheet. The method has the greatest advantages that the preparation process is simple, the ultrathin slice with high purity can be obtained, but the dimension is not easy to control and the repeatability is poor in the stripping process, and the yield of the prepared product is extremely low. (2) lithium ion intercalation method. In the method, lithium is used as an anode of a battery in a lithium ion battery device, a two-dimensional crystal is used as a cathode, lithium ions are intercalated into a two-dimensional material layer in a discharging process to form a lithium intercalation compound, the lithium intercalation compound reacts vigorously in water or ethanol solvent to generate a large amount of hydrogen to increase the interlayer spacing, and finally, the single-layer and less-layer layered material is obtained by stripping. The method can obtain a thin layer material with higher purity, but the size of the obtained material is not easy to control, and the method is difficult to be a main method for preparing a superconducting integrated circuit material. (3) liquid phase stripping method. The method is generally carried out by mixing a bulk of the two-dimensional crystalline material with a suitable solvent such as ethanol, N, N-Dimethylformamide (DMF) or N-methylpyrrolidone (NMP) and sonicating, wherein the sonicating breaks the interlayer Van der Waals forces of the two-dimensional material and the compatible surfaces of the solvent and the two-dimensional material allow the exfoliated platelets to be uniformly dispersed in the solvent. The liquid phase stripping method has simple operation method and can prepare low-dimensional nano sheets in a large scale, but long-time ultrasonic treatment can lead the obtained nano sheets to be small in size, and organic solvents are often used in the ultrasonic process to have great damage effect on the nano sheets, so that the method is difficult to be suitable for superconducting integrated circuits. (4) chemical vapor deposition. The method mainly utilizes vapor pressure generated by melting metal oxide and salt particles at high temperature to react with hydrogen sulfide/hydrogen selenide/hydrogen telluride, and performs nucleation growth on a substrate. The method can obtain a large-area film material, but the material performance of the material is seriously degraded after being processed by a micro-nano processing technology, and the limitation severely limits the application of the material on a superconducting integrated circuit.
In summary, there are often great limitations in the current preparation of superconducting materials. Conventional device fabrication processes can damage two-dimensional superconducting materials, including their electrical properties and surface structures. Therefore, it is important to find a suitable preparation method of the superconducting nano integrated circuit.
Disclosure of Invention
The invention aims to: the invention aims to provide a nondestructive preparation method of a two-dimensional superconducting nano integrated circuit, which has stable processing process and does not damage the electrical property and the structural surface of a two-dimensional superconducting material.
The technical scheme is as follows: the invention relates to a nondestructive preparation method of a two-dimensional superconducting nano integrated circuit, which comprises the following steps: firstly, growing an ultrathin transition metal film on a substrate; then, the nano integrated circuit device of the superconducting metal film is obtained by electron beam exposure and reactive ion etching; then, the metal film nano device is converted into a nano integrated device of a two-dimensional superconducting film in situ by using a topological chemical conversion method; and finally, growing a layer of insulating material on the device to obtain the two-dimensional superconducting nano integrated circuit.
In the scheme, the metal film nano device is directly converted into the nano integrated device of the two-dimensional superconducting film in situ without transferring the two-dimensional superconducting film, and the prepared two-dimensional superconducting film has few defects and excellent electrical property of the nano circuit.
Preferably, the metal film material is Nb, ti, ta, mo or a W metal thin layer.
Preferably, the substrate is Si, siO 2 Or Si (or) 3 N 4 A substrate.
Preferably, the insulating material is SiO 2 、Si 3 N 4 Or Al 2 O 3 。
As a further improvement of the above solution, the method specifically comprises the steps of:
(1) And (3) substrate treatment: before a metal film is grown, firstly, soaking a substrate in a piranha solution, then, carrying out high-temperature treatment in an oxygen atmosphere, thereby forming a step with a step shape on the substrate, and cleaning to obtain the substrate required by the film growth;
(2) And (3) growing a metal film: growing an ultrathin metal film at high temperature in magnetron sputtering to obtain a metal film with thin layer thickness, and then placing the metal film in a vacuum drying oven;
(3) Manufacturing a metal electrode: photoetching, gold growing and stripping the obtained metal film to obtain an electrode pattern with the metal film;
(4) Electron beam exposure: spin-coating electron beam glue on the metal film electrode, then exposing a nanowire area by utilizing EBL, and then developing to obtain a nanostructure pattern obtained by the electron beam glue;
(5) Preparing a nano circuit: placing the film in RIE for etching, and transferring the pattern formed by the electron beam glue to the metal film;
(6) Removing photoresist: placing the obtained metal pattern in an organic solvent for soaking in a water area to remove the residual electron beam glue on the surface, thereby obtaining a clean metal film pattern;
(7) Topological chemical conversion: placing the metal film pattern in a CVD system, and annealing in a reactive gas to obtain a high-quality two-dimensional superconducting material device pattern;
(8) And (3) growth of a packaging layer: and (3) growing an insulating layer on the two-dimensional superconducting material device pattern to obtain a packaged two-dimensional superconducting thin film material device, namely the two-dimensional superconducting nano integrated circuit.
As a further improvement of the scheme, in the step (1), the piranha solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide, the reaction temperature of soaking treatment is 150 ℃, and the reaction time is 30min; the high temperature treatment temperature is 1100 ℃, and the annealing time is 2-4 h.
As a further improvement of the above scheme, in the step (1), the cleaning method is to sequentially clean in acetone, ethanol and water for a period of time.
Preferably, in the step (2), the thickness of the metal film is about 1 to 2nm.
As a further improvement of the above scheme, in the step (3), the manufacturing of the metal electrode specifically includes the following steps:
a. spin-coating positive photoresist on the surface of the nano film layer;
b. patterning and exposing the positive photoresist;
c. developing and fixing to obtain a positive photoresist mask with an electrode shape;
d. depositing on the mask to obtain an electrode layer;
e. and preparing the metal electrode by using a lift-off process.
As a further improvement of the above-mentioned scheme, in the step (4), the electron beam exposure specifically includes the steps of:
a. spin-coating negative electron beam exposure glue on the surface of the nano film layer;
b. obtaining nanowire patterns by adopting an electron beam exposure method;
c. developing and fixing to obtain the electron beam exposure glue mask with nanowire shape.
Preferably, the gold electrode has a thickness of about 100nm.
Preferably, in the step (5), the pattern formed by the electron beam glue is formed by arranging a plurality of nanowires or other nano unit arrays, wherein the nanowires are serpentine nanowires, and the nanowire unit arrays are circular hole arrays, triangular arrays or spiral lines.
As a further improvement of the above-described scheme, in step (7), the in-reactive-gas annealing includes the steps of: a. placing S, se or Te powder at the front end of CVD;
b. heating according to S, se or Te powder to reach the melting point;
c. by simultaneous use of Ar/H 2 The mixed gas is used as carrier gas to bring S, se or Te to the upper part of the film and react with the film;
d. the required high temperature is 600-800 ℃.
Preferably, if Se powder is placed at the front end of CVD, the heating temperature is 300-450 ℃.
Preferably, in the step (7), the temperature rise rate of the CVD system is 20 ℃/min and the gas flow rate is 50sccm to 200sccm.
The invention designs a complete technical scheme for processing devices of two-dimensional superconducting materials. The technical scheme combines a topological chemical conversion method, thereby realizing the preparation of the device of the nondestructive two-dimensional superconducting material, and the method can realize the preparation of devices of various materials (including all two-dimensional materials), and provides a feasible scheme for the application of the two-dimensional materials on the micro-nano device.
The technical scheme provided by the invention not only can realize the preparation of a large-area superconducting nano integrated circuit, but also overcomes the defect that the traditional two-dimensional superconducting device is difficult to prepare in a large area, and the two-dimensional material prepared by the traditional method can only be in a micron level, so that the preparation of an inch-level device is difficult to realize, and the problem of how to make the size of a sample large is always solved in the field; in addition, the topological chemical conversion method provided by the invention can transfer the damage on the process to the precursor of the metal film preferentially, so that the damage of the micro-nano processing technology to the superconducting device can be completely avoided, the preparation of a large-area superconducting integrated circuit can be realized, and the traditional superconducting film does not show the superconducting property after the micro-nano processing technology due to the very high requirement of the superconducting property on the material, so that the two-dimensional superconducting material is difficult to run out of a laboratory.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages:
(1) The technical scheme provided by the invention can prepare various nano devices on the premise of not damaging the electrical property and the structural surface of the two-dimensional superconducting material, and avoids the damage effect of the traditional micro-nano technology on the devices.
(2) The technical scheme provided by the invention overcomes the problem of instability of the traditional two-dimensional material in micro-nano processing.
(3) The technical scheme provided by the invention can realize the preparation of the integrated circuit of the two-dimensional superconducting material in inch level, and overcomes the great difficulty that the prior two-dimensional material is difficult to go to practical application.
(4) Due to the personalized customization characteristics of the EBL, different device structures can be prepared on different substrates, so that the programmable application of different two-dimensional superconducting circuits is realized, and the two-dimensional superconducting materials and the technical scheme of device processing of the two-dimensional materials are perfected.
Drawings
Fig. 1 is a flow chart of a nondestructive fabrication method of a two-dimensional superconducting nano integrated circuit according to an embodiment of the present invention.
FIG. 2 is a schematic growth diagram of a topological chemical conversion process according to an embodiment of the invention.
Fig. 3 is a process flow diagram of a method for the non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to an embodiment of the present invention.
FIG. 4 is a two-dimensional superconducting NbSe of example 1 2 AFM image of nanodevices.
FIG. 5 is a view of NbSe prepared in example 1 and comparative example 1 2 The electrical properties of the devices were compared.
FIG. 6 is a two-dimensional superconducting NbS in example 3 2 AFM and raman images of nano-devices.
FIG. 7 is a two-dimensional superconducting TiSe in example 4 2 AFM and raman images of nano-devices.
FIG. 8 is a two-dimensional superconducting MoTe in example 5 2 Nanometer scaleAFM and raman images of the device.
FIG. 9 is a two-dimensional superconducting NbSe of different thickness and width in example 6 2 AFM image of nanodevices.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
As shown in FIG. 1, the implementation of the present invention provides a nondestructive fabrication method of a two-dimensional superconducting nano integrated circuit, which mainly comprises: a. growing a metal film; b. preparing a nano integrated device of a metal film; c. the metal thin film nano device is converted into a transition metal chalcogenide nano device; d. and (5) growing an insulating packaging layer. (wherein the substrate is alumina, the metal film material is Nb, and the two-dimensional superconducting material is NbSe 2 )。
As shown in fig. 1-3, the embodiment of the invention provides a specific process flow of a nondestructive preparation method of a two-dimensional superconducting nano integrated circuit, which comprises the following steps:
(1) And (5) treating a substrate. The substrate used is alumina (the substrate size is not particularly required and can be 1inch,2inch and other sizes). Before using the substrate, the substrate is firstly placed in a piranha solution (concentrated sulfuric acid: hydrogen peroxide=7:3) for treatment for 30min, then the substrate is calcined at high temperature for 4h (1100 ℃) in an oxygen environment, then the substrate is respectively treated in acetone, ethanol and water for 10min, and finally the substrate is dried by a nitrogen gun and placed in a drying cabinet.
(2) And growing a metal film. The substrate was placed in a high vacuum system for magnetron sputtering, and a process gas flow rate of 100sccm (Ar gas), an operating gas pressure of 0.27Pa, and an operating power of 100W were selected. Under this growth condition, the deposition rate of the metallic Nb film is close to 0.4nm/s. The growth time is controlled to be 5s, and a metal thin film layer with the thickness of about 2nm (namely, shown in the figure 1 a) can be obtained.
(3) And (5) manufacturing a metal electrode. The film is placed on a spin-coating machine, a layer of photoresist is spin-coated, the rotating speed is 4000rpm, the acceleration is 2000rpm/s, and the spin-coating time is 40s. Then exposing by using 385nm ultraviolet photoetching machine, exposing the metal film after developing, and protecting the unexposed place by photoresist. Next, the developed sample was placed in magnetron sputtering to grow a titanium gold electrode with a thickness of about 100nm. The conditions for growing the titanium electrode are as follows: the flow rate of the process gas was 80sccm (Ar gas), the operating gas pressure was 0.36Pa, and the operating power was 80W.
The end of the growing electrode then requires a lift-off process. That is, the metal electrode is covered on the exposed metal film after development, and the photoresist remained on the unexposed place is very soluble in acetone, so that the sample is placed in the acetone solution for ultrasonic treatment for 20min (the ultrasonic power is 100W), and the designed pattern of the metal electrode can be obtained.
(4) And E, electron beam exposure. The sample is spin coated with a layer of electron beam positive resist (PMMA) and then placed in an electron beam exposure system for exposure treatment. The principle of the electron beam positive photoresist is basically consistent with that of the photoresist, namely, the exposed places are removed, and the unexposed places remain on the protective metal film. After the exposure and development steps, our electron beam resist is converted into a pattern of nano-circuits.
(5) Reactive Ion Etching (RIE) prepares the nanocircuit. The pattern is placed in a reaction chamber of the RIE, the exposed area of the metal film is etched completely after exposure, and the unexposed area is protected by the electron beam glue. The process formula in the process is as follows: etching power 100W, etching gas CF 4 The gas flow rate was 40sccm, the other working pressure was 4Pa, and the etching time was 20s.
(6) And (5) removing photoresist. After etching, the electron beam glue is still protected, so that the residual electron beam glue is removed after the water area treatment of N methyl at 80 ℃ for 30 min.
The metal thin film is thus converted into thin film nanowires after the above steps (i.e. as shown in fig. 1 b).
(7) Topologically transformed CVD anneal. Placing the thin film nanowire structure horizontally in a CVD system, placing 2g of selenium powder at 15cm of the front end of the thin film nanowire structure, and vacuumizing by a mechanical pump1Pa or less (schematic view is shown in FIG. 2). Then argon-hydrogen mixture gas is introduced to normal pressure, the CVD system is heated to 800 ℃, and the high temperature and the normal pressure are maintained for 15 minutes to realize the topological transformation from the metal film material to the transition metal chalcogenide (as shown in figure 1 c). The technological parameter conditions are as follows: se powder temperature: 400 ℃, metal film reaction temperature: 800 ℃, reaction flow: ar: H 2 =80:20 sccm, reaction time: 15min.
(8) And (5) growing an encapsulation layer. In a PECVD system, the sample is placed under vacuum of 5.1X10 times -1 Pa, subsequent growth of Si close to 50nm 3 N 4 Encapsulation layer (as shown in fig. 1 d). The reaction parameters are as follows: siH (SiH) 4 /N 2 :NH 3 :N 2 =100:6:100 sccm, reaction temperature: 300 ℃, working air pressure: 80Pa, growth power: 40W, the growth rate was approximately 0.3nm/s.
As shown in FIG. 4, nbSe prepared in this example 2 A macroscopic view of the nanowire device structure and its corresponding AFM view. The graph can prove that the method of the embodiment can not only realize the preparation of the two-dimensional superconducting device with the inch grade, but also ensure that the surface of the device is quite clean and smooth, and the boundaries of adjacent nanowires are obvious and the edges are sharp.
Comparative example 1
This comparative example provides a method of manufacturing a nanowire device, which is different from example 1in that: in the step (2), a CVD system is adopted to grow a two-dimensional superconducting film, which concretely comprises the following steps:
(1) And (5) treating a substrate. The substrate used is alumina (the substrate size is not particularly required and can be 1inch,2inch and other sizes). Before using the substrate, the substrate is firstly placed in a piranha solution (concentrated sulfuric acid: hydrogen peroxide=7:3) for treatment for 30min, then the substrate is calcined at high temperature for 4h (1100 ℃) in an oxygen environment, then the substrate is respectively treated in acetone, ethanol and water for 10min, and finally the substrate is dried by a nitrogen gun and placed in a drying cabinet.
(2) And growing a two-dimensional superconducting film. Inverting the substrate and placing 5g of Nb under the substrate in a sample boat 2 O 5 Powder and 0.5g NaCl powder, then the sample boat was placed in a CVD systemIn the system. And placing 2g of selenium powder at 15cm of the front end of the container, and pumping vacuum to below 1Pa by a mechanical pump. Then introducing argon-hydrogen mixture gas to normal pressure, heating the CVD system to 800 ℃, and keeping the high temperature and normal pressure for 15min to realize the two-dimensional superconducting film NbSe 2 Is prepared by the following steps. The technological parameter conditions are as follows: se powder temperature: 400 ℃, reaction temperature: 800 ℃, reaction flow: ar: H 2 =80:20 sccm, reaction time: 15min.
(3) And (5) manufacturing a metal electrode. The film is placed on a spin-coating machine, a layer of photoresist is spin-coated, the rotating speed is 4000rpm, the acceleration is 2000rpm/s, and the spin-coating time is 40s. Then, a 385nm ultraviolet photoetching machine is used for carrying out fixed-point area exposure, the exposed part exposes the metal film after development, and the unexposed part is still protected by photoresist. Next, the developed sample was placed in magnetron sputtering to grow a titanium gold electrode with a thickness of about 100nm. The conditions for growing the titanium electrode are as follows: the flow rate of the process gas was 80sccm (Ar gas), the operating gas pressure was 0.36Pa, and the operating power was 80W.
The end of the growing electrode then requires a lift-off process. That is, the metal electrode is covered on the exposed metal film after development, and the photoresist remained on the unexposed place is very soluble in acetone, so that the sample is placed in N-methyl pyrrolidone solution for 30min in a high-temperature (80 ℃) water area, and the designed pattern of the metal electrode can be obtained.
(4) And E, electron beam exposure. The sample is spin coated with a layer of electron beam positive resist (PMMA) and then placed in an electron beam exposure system for exposure treatment. The principle of the electron beam positive photoresist is basically consistent with that of the photoresist, namely, the exposed places are removed, and the unexposed places remain on the protective metal film. After the exposure and development steps, our electron beam resist is converted into a pattern of nano-circuits.
(5) Reactive Ion Etching (RIE) prepares the nanocircuit. The pattern is placed in a reaction chamber of RIE, the exposed area of the metal film is etched completely after exposure, and the unexposed area is provided with the electron beam glue to cause the metal filmIs protected. The process formula in the process is as follows: etching power 100W, etching gas CF 4 The gas flow rate was 40sccm, the other working pressure was 4Pa, and the etching time was 20s.
(6) And (5) removing photoresist. After etching, the electron beam glue is still reserved on the surface of the wafer, so that the wafer needs to be treated in a water area of N methyl at 80 ℃ for 30min, and the residual electron beam glue is removed completely, so that the required device structure can be obtained.
(7) And (5) growing an encapsulation layer. In a PECVD system, the sample is placed under vacuum of 5.1X10 times -1 Pa, subsequent growth of Si close to 50nm 3 N 4 Encapsulation layer (as shown in fig. 1 d). The reaction parameters are as follows: siH (SiH) 4 /N 2 :NH 3 :N 2 =100:6:100 sccm, reaction temperature: 300 ℃, working air pressure: 80Pa, growth power: 40W, the growth rate was approximately 0.3nm/s.
Fig. 5 shows a comparative graph of the device prepared using example 1 and the device prepared using comparative example 1. As can be seen from the graph, the performance of the device prepared using example 1 is greatly improved over that of comparative example 1. In which figure 5a shows the atomic photoelectron spectrum of Nb. As can be seen from the figure, nbSe prepared by the method of example 1 2 The weak peak of niobium oxide in the nanocircuit, i.e. the oxidation of the material in the process, means that the method belongs to a non-destructive processing method. In addition, FIG. 5b shows the atomic photoelectron spectrum of Se, as can be seen, likewise, nbSe prepared by the implementation of example 1 2 Fewer Se-O bonds in the nanocircuit also means fewer defects are generated in the process. In addition, FIG. 5c shows NbSe prepared using example 1 2 The electrical performance of the nanocircuit is significantly better than the method of comparative example 1. NbSe prepared by the method of example 1 2 The nanocircuit is capable of exhibiting a complete superconducting IV curve at low temperatures, whereas the device prepared using the method of comparative example 1 is difficult to exhibit an IV curve. This also means that the devices produced by the present route of technology belong to a non-destructive processing production method.
Example 2
The present embodiment provides a two-dimensional superconductiveThe non-destructive preparation method of the integrated circuit is basically the same as that of example 1, except that: in step (8), the encapsulation layer is replaced by SiO 2 . The technological parameters are as follows: siH (SiH) 4 /N 2 :N 2 O:N 2 =80:120:40 sccm, reaction temperature: 300 ℃, working air pressure: 100Pa, growth power: 15W, the growth rate was approximately 0.6nm/s.
Example 3
This example provides a nondestructive fabrication method of a two-dimensional superconducting nano integrated circuit, which utilizes the technical route of the present invention to achieve the preparation of different metal chalcogenides, and the method of this example is basically the same as that of example 1, except that: in the step (7), the reacted Se powder is replaced with S powder in the process of utilizing topological chemical conversion, and the reaction temperature of the S powder is 300 ℃. NbS realized by the method of the embodiment 2 AFM and raman spectra corresponding to the nanopore device structure are shown in fig. 6. From the spectra, it can be known that the grown NbS 2 The size of the nano holes is basically consistent, and the maturity and feasibility of the device prepared by the technical route are also verified.
Example 4
This example provides a nondestructive fabrication method of a two-dimensional superconducting nano integrated circuit, which utilizes the technical route of the present invention to achieve the preparation of different metal chalcogenides, and the method of this example is basically the same as that of example 1, except that: in the step (2), the metal thin film Nb film is replaced with a metal Ti film. The technological parameters of Ti film growth are as follows: working gas: ar=100 sccm, working gas pressure: 0.36Pa, working current: 0.4A, growth rate is: 0.3nm/s and the growth time is 6s. TiSe realized by the method of the embodiment 2 AFM and raman spectra corresponding to nanowire device structures as shown in fig. 7. From the spectrum, it can be known that the grown TiSe 2 The nanowire is subjected to AFM test, the color is uniform, and the Raman peak A 1g Peak sum E 1g The peaks all show that the devices produced using this method are of very high quality.
Example 5
The present embodiment provides a two-dimensional structureA method for the non-destructive preparation of superconducting nano-integrated circuits, which uses the technical route of the present invention to achieve the preparation of different metal chalcogenides, the method of the examples being substantially identical to that of example 1, except that: in the step (2), the metal film Nb film is replaced by a metal Mo film, and in the step (7), the Se source is replaced by a Te source. The technological parameters of the Mo film growth are as follows: working gas: ar=50 sccm, working gas pressure: 0.9Pa, operating voltage: 50W, the growth rate is: 0.15nm/s, and the growth time is 15s. In addition, the temperature of Te powder in the process of recycling topological chemical conversion is 500 ℃. MoTe realized by using the technical route 2 AFM and raman spectra corresponding to the helix device structure of (a) are shown in fig. 8. From the map, it can be known that the grown MoTe 2 The spiral line has uniform width and sharp Raman peak, and the technical route is proved to be capable of realizing the preparation of various two-dimensional superconducting circuits such as S/Se/Te with different elements.
Example 6
The present embodiment provides a nondestructive fabrication method of a two-dimensional superconducting nano integrated circuit, which is substantially identical to embodiment 1, and differs from embodiment 1 only in that: the thickness, width, pattern and pattern pitch of the nanowires can be custom-defined for the user, as shown in fig. 9.
Claims (10)
1. A method for the non-destructive fabrication of a two-dimensional superconducting nano integrated circuit, the method comprising the steps of: firstly, growing an ultrathin transition metal film on a substrate; then, the nano integrated circuit device of the superconducting metal film is obtained by electron beam exposure and reactive ion etching; then, the metal film nano device is converted into a nano integrated device of a two-dimensional superconducting film in situ by using a topological chemical conversion method; and finally, growing a layer of insulating material on the device to obtain the two-dimensional superconducting nano integrated circuit.
2. The method for non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein the metal thin film material is a Nb, ti, ta, mo or W metal thin layer.
3. The method for the non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein the substrate is Si, siO 2 Or Si (or) 3 N 4 A substrate; or the insulating material is SiO 2 、Si 3 N 4 Or Al 2 O 3 。
4. The method for the non-destructive preparation of a two-dimensional superconducting nano integrated circuit according to claim 1, characterized in that it comprises in particular the following steps:
(1) And (3) substrate treatment: before a metal film is grown, firstly, soaking a substrate in a piranha solution, then, carrying out high-temperature treatment in an oxygen atmosphere, thereby forming a step with a step shape on the substrate, and cleaning to obtain the substrate required by the film growth;
(2) And (3) growing a metal film: growing an ultrathin metal film at high temperature in magnetron sputtering to obtain a metal film with thin layer thickness, and then placing the metal film in a vacuum drying oven;
(3) Manufacturing a metal electrode: photoetching, gold growing and stripping the obtained metal film to obtain an electrode pattern with the metal film;
(4) Electron beam exposure: spin-coating electron beam glue on the metal film electrode, then exposing a nanowire area by utilizing EBL, and then developing to obtain a nanostructure pattern obtained by the electron beam glue;
(5) Preparing a nano circuit: placing the film in RIE for etching, and transferring the pattern formed by the electron beam glue to the metal film;
(6) Removing photoresist: placing the obtained metal pattern in an organic solvent for soaking in a water area to remove the residual electron beam glue on the surface, thereby obtaining a clean metal film pattern;
(7) Topological chemical conversion: placing the metal film pattern in a CVD system, and annealing in a reactive gas to obtain a high-quality two-dimensional superconducting material device pattern;
(8) And (3) growth of a packaging layer: and (3) growing an insulating layer on the two-dimensional superconducting material device pattern to obtain a packaged two-dimensional superconducting thin film material device, namely the two-dimensional superconducting nano integrated circuit.
5. The method for non-destructive production of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in the step (1), the piranha solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide.
6. The method for non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in step (1), the cleaning method is a cleaning in acetone, ethanol and water sequentially for a period of time.
7. The method for non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in step (3), the fabrication of the metal electrode specifically comprises the steps of:
a. spin-coating positive photoresist on the surface of the nano film layer;
b. patterning and exposing the positive photoresist;
c. developing and fixing to obtain a positive photoresist mask with an electrode shape;
d. depositing on the mask to obtain an electrode layer;
e. and preparing the metal electrode by using a lift-off process.
8. The method for the non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in step (4), the electron beam exposure specifically comprises the steps of:
a. spin-coating negative electron beam exposure glue on the surface of the nano film layer;
b. obtaining nanowire patterns by adopting an electron beam exposure method;
c. developing and fixing to obtain the electron beam exposure glue mask with nanowire shape.
9. The method for non-destructive fabrication of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in step (5), the pattern formed by the electron beam glue is formed by arranging a plurality of nanowires or other nano-element arrays, wherein the nanowires are serpentine nanowires, and the nanowire element arrays are circular hole arrays, triangular arrays or spiral lines.
10. The method for the non-destructive production of a two-dimensional superconducting nano integrated circuit according to claim 1, wherein in step (7), the reactive gas annealing comprises the steps of: a. placing S, se or Te powder at the front end of CVD;
b. heating according to S, se or Te powder to reach the melting point;
c. by simultaneous use of Ar/H 2 The mixed gas is used as carrier gas to bring S, se or Te to the upper part of the film and react with the film;
d. the required high temperature is 600-800 ℃.
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