CN116536628B - Method for preparing nano-scale amorphous superconducting film by utilizing magnetron sputtering and product - Google Patents
Method for preparing nano-scale amorphous superconducting film by utilizing magnetron sputtering and product Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 42
- 238000004544 sputter deposition Methods 0.000 claims abstract description 82
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 34
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3492—Variation of parameters during sputtering
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- 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
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Abstract
The invention provides a method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering and a product thereof, belonging to the technical field of superconducting films, wherein the method comprises the following steps: and sputtering for 10min-3h with sputtering power of 30-60W in an argon environment by utilizing magnetron sputtering, and depositing a target Mo80Nb20 on the Si substrate to obtain the nanoscale amorphous superconducting film. The invention also discloses the nano-scale amorphous superconducting film prepared by the method. The invention simplifies the preparation process and reduces the cost by adjusting the power and the sputtering time in the sputtering process, and the prepared Mo80Nb20 nanoscale amorphous superconducting film has uniform thickness distribution and stable quality and structure. The Mo80Nb20 nanoscale amorphous superconducting film prepared by the method has higher critical transition temperature and obvious thickness correlation.
Description
Technical Field
The invention belongs to the technical field of superconducting films, and particularly relates to a method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering and a product.
Background
The quantum information technology has become a high point of future technologies, with the development of integrated circuits, the research of conductor resistivity has reached a size effect mechanism, the superconducting quantum chip is manufactured and popularized and applied, and the research of basic materials is important, wherein the superconducting materials are breakthrough points. The breakthrough progress and widespread use of superconducting technology will have immeasurable impact on technological, economic, military and even social developments. The method has unlimited application prospects in the fields of power transmission, motors, aerospace, microelectronics, electronic computers, communication and the like. The application of the superconducting material can not only improve the working efficiency, but also greatly save energy sources and reduce a great amount of pollution.
The metallic glass, also called amorphous alloy, has long-range disordered atomic structure and short-range ordered atomic structure, and has excellent mechanical, chemical and physical properties. In 1954, amorphous superconducting films of bismuth and gallium were obtained on a liquid helium cooled plate by vacuum evaporation, after which amorphous superconductors of strips or flakes of Pd-Zr, zr-Ni-Cu, nb-Ge, etc. were subsequently found. It has also been found in the prior art that metallic glass electrical transport properties change significantly as the physical dimensions of the conductor approach or are smaller than the intrinsic electron mean free path, for example, the superconducting transition temperature of bulk Mo metal is 0.9K, which is as high as 9.8K after fabrication into a thin film, and in superlattice lattice, nb decreases from 9.2K to 2K as disordered structure is replaced, while Mo increases from 0.9K to 8K as disordered. Thus, it may be advantageous to obtain films with higher superconducting transition temperatures by reducing the size and increasing the disorder.
In the process of preparing the nano-scale amorphous superconducting thin film, cooling is required to be performed in a short time, and meanwhile, the nano-scale thin film thickness is required to be met. The common amorphous film preparation methods in the prior art mainly comprise physical vapor deposition methods such as a magnetron sputtering method, ion plating, ion beam assisted deposition, electron beam evaporation method and the like, chemical vapor deposition methods and the like. The magnetron sputtering technology can be used for preparing various materials such as metal, semiconductor, insulator and the like, and has the advantages of simple equipment, easy control, large film plating area and the like, but the magnetron sputtering technology in the prior art is used for preparing the film often needs higher sputtering power or sputtering temperature, and the quality of the finally obtained film product is lower.
Therefore, how to optimize the method for preparing the nano-scale amorphous superconducting film by using the magnetron sputtering technology in the prior art is a technical problem to be solved by the skilled person.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering and a product thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
sputtering for 10min-3h with sputtering power of 30-60W in an argon environment, and depositing a target Mo80Nb20 on the Si substrate and the glass sheet to obtain the nanoscale amorphous superconducting film.
The beneficial effects are that: the invention prepares the nano-scale Mo80Nb20 amorphous superconducting film by utilizing magnetron sputtering, controls the film thickness by controlling the sputtering time, and obtains the nano-scale amorphous superconducting film with higher superconducting transition temperature, and has low preparation cost and simple process flow.
Preferably, the purity of the target Mo80Nb20 is higher than 99.95%, and the substrate is Si (100).
The beneficial effects are that: the purity of the target material has great influence on the performance of the sputtering film, and the higher the purity of the target material is, the better the performance of the sputtering film is, and the invention selects Mo80Nb20 with the purity of more than 99.95 percent as the target material, so that the performance of the sputtering film is not influenced by impurities.
Preferably, the magnetron sputtering method further comprises target pretreatment and substrate pretreatment.
The beneficial effects are that: the sputtering effect can be greatly improved by preprocessing the target material and the bottom before magnetron sputtering, so that the film performance is prevented from being influenced by the surface defects of the target material and the substrate.
Preferably, the target pretreatment includes the following steps:
polishing the oxide layer on the surface of the target, placing the target in absolute ethyl alcohol and deionized water, performing ultrasonic cleaning, and drying.
The beneficial effects are that: the oxide layer on the target surface affects the purity of the sputtered film and therefore needs to be removed.
Preferably, the substrate pretreatment includes the steps of:
and ultrasonically cleaning the substrate in absolute ethyl alcohol and deionized water, and then drying.
The beneficial effects are that: dust and stains on the substrate surface introduce impurities into the sputtered film, affecting its performance, and therefore need to be removed cleanly.
Preferably, the vacuum condition is: firstly, using a mechanical pump to vacuumize until the pressure is below 5Pa, and then using a molecular pump to vacuumize until the pressure is below 8 multiplied by 10 -4 Pa。
The beneficial effects are that: during sputtering, oxygen in the chamber oxidizes the sputtered film, thus requiring a chamber vacuum of less than 8×10 -4 Pa to reduce the oxygen content in the chamber.
Preferably, the vacuum degree during the sputtering is lower than 8×10 -4 And after Pa, introducing argon, keeping the flow of the argon gas at 55-65sccm, and keeping the working air pressure at 0.5Pa-1.2Pa by adjusting a molecular pump valve, wherein the temperature is room temperature.
The beneficial effects are that: the invention is introduced with argon to ensure the anaerobic environment of the cavity and simultaneously provides high-energy particles for bombarding the target material.
Preferably, the pre-sputtering further comprises pre-sputtering, and the pre-sputtering time is 30min.
The beneficial effects are that: an oxide film exists on the surface of the target material, and sputtering is carried out after the oxide film is removed.
A nano-scale amorphous superconducting film prepared by a method for preparing the nano-scale amorphous superconducting film by utilizing magnetron sputtering.
The beneficial effects are that: the Mo80Nb20 nano-scale amorphous superconducting film prepared by the method has uniform thickness distribution and stable quality and structure. The Mo80Nb20 nano-scale amorphous superconducting film has higher critical transition temperature and obvious thickness dependence.
Preferably, the nanoscale superconducting thin film is of an amorphous structure and has a thickness of 30-900nm;
the nano-scale superconducting film has a superconducting transition phenomenon at a low temperature, and the superconducting transition temperature is 4.4-5.9K.
The beneficial effects are that: the Mo80Nb20 nano-scale amorphous superconducting transition temperature prepared by the method is up to 5.9K, and exceeds that of a common amorphous superconducting film.
The invention provides a method and a product for preparing a nano-scale amorphous superconducting film by utilizing magnetron sputtering, which can prepare the amorphous Mo80Nb20 nano-scale amorphous superconducting film at room temperature finally by adjusting the power and the sputtering time in the sputtering process, thereby simplifying the preparation process and reducing the cost. The invention can obtain Mo80Nb20 nano-scale amorphous superconducting films with different thicknesses by controlling the sputtering power and time, has simple operation and easy control, and the prepared Mo80Nb20 nano-scale amorphous superconducting film has uniform thickness distribution and stable quality and structure. The Mo80Nb20 nanoscale amorphous superconducting film prepared by the method has higher critical transition temperature and obvious thickness correlation.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application, illustrate and explain the application and are not to be construed as limiting the application. In the drawings:
FIG. 1 is a SEM surface morphology of the nano-scale amorphous superconducting thin films obtained in examples 1 and 5 of the present invention; wherein, (a) is the nanoscale amorphous superconducting film obtained in example 1, and (b) is the nanoscale amorphous superconducting film obtained in example 5;
FIG. 2 is a SEM sectional profile of the nano-scale amorphous superconducting thin films obtained in examples 1 and 5, and measurement of the thickness of the thin films; (a) A nanoscale amorphous superconducting film obtained in example 1, and (b) a nanoscale amorphous superconducting film obtained in example 5;
FIG. 3 is a surface topography of the film obtained in comparative example 4;
FIG. 4 (a) is an XRD pattern of the nano-scale amorphous superconducting thin film obtained in example 5, and (b) is an XRD pattern of the thin film obtained in comparative example 4;
FIG. 5 shows the superconducting transition temperature T of the nanoscale amorphous superconducting thin film obtained in examples 1 to 5 c ；
FIG. 6 is a graph showing the change in resistivity with temperature of the nanoscale films obtained in comparative examples 1 to 3.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
The Mo80Nb20 target used in the embodiment of the invention is purchased from Zaijin New material company, the purity is 99.95%, the diameter of the target is 50mm, and the thickness is 3-5mm;
the magnetron sputtering deposition system used in the embodiment of the invention is a JGP-450 type high vacuum magnetron sputtering system of Shenyang scientific instruments, inc. of Chinese academy of sciences;
the surface and the section of the Mo80Nb20 nanoscale amorphous superconducting film obtained in the embodiment of the invention are detected by a high-resolution field emission scanning electron microscope (HR-FESEM), and the model of the used equipment is as follows: ZEISS GeminiSEM 300;
the structure of the Mo80Nb20 nanoscale amorphous superconducting film obtained in the embodiment of the invention is detected by an X-ray diffractometer (XRD) and a high-resolution transmission electron microscope (HRTEM), and the model of XRD equipment is as follows: blaker D8 Discover, the model of the used HRTEM device is JEM-2100F;
the low-temperature resistance of the Mo80Nb20 nanoscale amorphous superconducting film obtained in the embodiment of the invention is tested by a comprehensive physical property testing system (PPMS) of Quantum Design company, and the model of the used equipment is PPMS-9T.
Example 1
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: polishing the surface of a Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, drying and fixing on a magnetron sputtering target head; and sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 When Pa, argon is introduced, the flow rate of the gas is controlled to be 60sccm, a direct current power supply is turned on after the pressure of a cavity is kept at 3Pa by controlling a molecular pump valve, the power is regulated to be 30W for starting, after the glow is stable, the working pressure of the molecular pump valve is regulated to be kept at 1Pa, and the pre-sputtering is carried out on a sample platform without a substrate for 30min;
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, turning off a direct current power supply after 10min, and obtaining the nanoscale amorphous superconducting film after the sputtering is over.
The technical effects are as follows:
1. the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by SEM, as shown in part (a) of fig. 1, the film surface is compact and uniform, and no obvious holes are formed.
2. The cross-sectional morphology of the sample prepared in step (3) was characterized by SEM and the thickness thereof was measured, as shown in part (a) of fig. 2, and the film thickness was 37nm.
3. The sample prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous, and a small amount of sharp small peaks exist, so that some nanocrystals can exist.
4. The low temperature resistance of the nano-scale amorphous superconducting film prepared in the step (3) is measured by PPMS, and fig. 4 shows the change curve of the resistance with temperature in this example, and it can be found that superconducting transformation occurs, and the superconducting transformation temperature is as high as 5.9K.
Example 2
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 When Pa, argon is introduced, the flow rate of the gas is controlled to be 60sccm, a direct current power supply is turned on after the pressure of a cavity is kept at 3Pa by controlling a molecular pump valve, the power is regulated to be 30W for starting, after the glow is stable, the working pressure of the molecular pump valve is regulated to be kept at 1Pa, and the pre-sputtering is carried out on a sample platform without a substrate for 30min;
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, turning off a direct current power supply after 30min, and obtaining the nanoscale amorphous superconducting film after sputtering is over.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, wherein the film surface is compact and uniform, and no obvious holes are formed.
2. And (3) characterizing the cross-sectional morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, and measuring the thickness of the nano-scale amorphous superconducting film to 104nm.
3. The structure of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous. There are a small number of sharp small peaks, indicating that some nanocrystals may be present.
4. The low temperature resistance of the sample prepared by sputtering in the above step 3 was measured by PPMS, and fig. 4 shows the change curve of the resistance with temperature of this example, the superconducting transition occurred, and the superconducting transition temperature was about 5.8K.
Example 3
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 When Pa, argon is introduced, the flow rate of the gas is controlled to be 60sccm, a direct current power supply is turned on after the pressure of a cavity is kept at 3Pa by controlling a molecular pump valve, the power is regulated to be 30W for starting, after the glow is stable, the working pressure of the molecular pump valve is regulated to be kept at 1Pa, and the pre-sputtering is carried out on a sample platform without a substrate for 30min;
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 1h, turning off a direct current power supply, and ending the sputtering to obtain the nanoscale amorphous superconducting film.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, wherein the film surface is compact and uniform, and no obvious holes are formed.
2. And (3) characterizing the cross-sectional morphology of the nano amorphous superconducting film prepared in the step (3) through SEM, and measuring the thickness of the nano amorphous superconducting film to be 286nm.
3. The structure of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous. There are a small number of sharp small peaks, indicating that some nanocrystals may be present.
4. The low temperature resistance of the sample prepared by sputtering in the above step 3 was measured by PPMS, and fig. 4 shows the temperature-dependent change curve of the resistance of the present example, the superconducting transition occurred, and the superconducting transition temperature was about 5.6K.
Example 4
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 When Pa, argon is introduced, the flow rate of the gas is controlled to be 60sccm, a direct current power supply is turned on after the pressure of a cavity is kept at 3Pa by controlling a molecular pump valve, the power is regulated to be 30W for starting, after the glow is stable, the working pressure of the molecular pump valve is regulated to be kept at 1Pa, and the pre-sputtering is carried out on a sample platform without a substrate for 30min;
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 2 hours, turning off a direct current power supply, and ending the sputtering to obtain the nanoscale amorphous superconducting film.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, wherein the film surface is compact and uniform, and no obvious holes are formed.
2. And (3) characterizing the cross-sectional morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, and measuring the thickness of the nano-scale amorphous superconducting film to 562nm.
3. The structure of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous. There are a small number of sharp small peaks, indicating that some nanocrystals may be present.
4. The low temperature resistance of the nano-scale amorphous superconducting film prepared in the step (3) is measured by PPMS, and fig. 4 shows the change curve of the resistance with temperature in this example, the superconducting transformation occurs, and the superconducting transformation temperature is about 5.3K.
Example 5
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 When Pa, argon is introduced, the flow rate of the gas is controlled to be 60sccm, a direct current power supply is turned on after the pressure of a cavity is kept at 3Pa by controlling a molecular pump valve, the power is regulated to be 30W for starting, after the glow is stable, the working pressure of the molecular pump valve is regulated to be kept at 1Pa, and the pre-sputtering is carried out on a sample platform without a substrate for 30min;
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 3 hours, turning off a direct current power supply, and ending the sputtering to obtain the nanoscale amorphous superconducting film.
The technical effects are as follows:
1. the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by SEM, as shown in part (b) of fig. 1, the film surface is compact and uniform, and no obvious holes are formed.
2. The nano-sized amorphous superconducting film prepared in the step (3) was characterized in its cross-sectional morphology by SEM, as shown in part (b) of fig. 2, and its thickness was measured to be 888nm.
3. The structure of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by XRD, as shown in figure 3, no obvious sharp strong peak exists, and the prepared film is mostly amorphous. There are a small number of sharp small peaks, indicating that some nanocrystals may be present. The inset is a corresponding selected area electron diffraction pattern, which can be seen to show a typical amorphous ring, which was verified to be amorphous by advances.
4. The low-temperature resistance of the nano-scale amorphous superconducting film prepared in the step (3) is measured by PPMS, the change curve of the resistance along with the temperature is shown in figure 4, the superconducting transformation is seen, and the superconducting transformation temperature is about 4.4K.
Example 6
A method for preparing a nanoscale amorphous superconducting film by utilizing magnetron sputtering comprises the following steps:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, sequentially opening a cooling water system, a total power supply, a mechanical pump valve and a vacuum indicator, closing the mechanical pump valve when the vacuum degree is lower than 5Pa, opening an isolation electromagnetic valve, a molecular pump power supply and a molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 Pa, lead toArgon is introduced, and the gas flow is controlled to be 60sccm. After the air pressure of the cavity is kept at 3Pa by controlling a molecular pump valve, a direct current power supply is turned on, the power is regulated to 60W for starting, after the glow is stable, the working air pressure of the molecular pump valve is kept at 1Pa, and the pre-sputtering is carried out on a sample table without a substrate for 30min.
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 1h, turning off a direct current power supply, and ending the sputtering to obtain the nanoscale amorphous superconducting film.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, wherein the film surface is compact and uniform, and no obvious holes are formed.
2. And (3) characterizing the cross-sectional morphology of the nano-scale amorphous superconducting film prepared in the step (3) through SEM, and measuring the thickness of the nano-scale amorphous superconducting film to 750nm.
3. The structure of the nano-scale amorphous superconducting film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous. There are a small number of sharp small peaks, indicating that some nanocrystals may be present.
4. And (3) measuring the low-temperature resistance of the nano amorphous superconducting film prepared in the step (3) by PPMS, wherein superconducting transformation occurs, and the superconducting transformation temperature is about 4.7K.
Comparative example 1
A method of Mo80Nb20 film comprising the steps of:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, and sequentially opening a cooling water system, a main power supply, a mechanical pump valve and a vacuum readingAnd (3) when the vacuum degree is lower than 5Pa, closing the mechanical pump valve, opening the isolation electromagnetic valve, the molecular pump power supply and the molecular pump valve, and vacuumizing until the vacuum degree is lower than 8 multiplied by 10 -4 Argon is introduced during Pa, and the gas flow is controlled to be 60sccm. After the air pressure of the cavity is kept at 3Pa by controlling a molecular pump valve, a direct current power supply is turned on, the power is adjusted to 15W for starting, after the glow is stable, the working air pressure of the molecular pump valve is kept at 1Pa, and the pre-sputtering is carried out on a sample table without a substrate for 30min.
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, turning off a direct current power supply after 10min, and obtaining the Mo80Nb20 film after the sputtering is over.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the Mo80Nb20 film prepared in the step (3) through SEM, wherein the film surface is compact and uniform and has no obvious holes.
2. The cross-sectional morphology of the Mo80Nb20 film prepared in the step (3) is characterized by SEM, and the thickness of the film is measured to be 30nm.
3. The structure of the Mo80Nb20 film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous.
4. And (3) measuring the low-temperature resistance of the Mo80Nb20 film prepared in the step (3) by PPMS, wherein no superconducting transformation occurs.
Comparative example 2
A method of Mo80Nb20 film comprising the steps of:
(1) Pretreatment: and (3) polishing the surface of the Mo80Nb20 target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2) Putting a baffle plate into the sputtering device, closing the cavity, and then sequentially opening a cooling water system, a main power supply, a mechanical pump power supply and a mechanical pumpValve and vacuum indicator, when the vacuum degree is lower than 5Pa, closing the mechanical pump valve, and opening the isolation electromagnetic valve, molecular pump power supply and molecular pump valve, and vacuumizing until the vacuum degree is lower than 8×10 -4 Argon is introduced during Pa, and the gas flow is controlled to be 60sccm. After the air pressure of the cavity is kept at 3Pa by controlling a molecular pump valve, a direct current power supply is turned on, the power is adjusted to 15W for starting, after the glow is stable, the working air pressure of the molecular pump valve is kept at 1Pa, and the pre-sputtering is carried out on a sample table without a substrate for 30min.
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, turning off a direct current power supply after 30min, and obtaining the Mo80Nb20 film after the sputtering is over.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the Mo80Nb20 film prepared in the step (3) through SEM, wherein the film surface is compact and uniform and has no obvious holes.
2. The cross-sectional morphology of the Mo80Nb20 film prepared in the step (3) is characterized by SEM, and the thickness of the film is measured to be 65nm.
3. The structure of the Mo80Nb20 film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous.
4. And (3) measuring the low-temperature resistance of the Mo80Nb20 film prepared in the step (3) by PPMS, wherein no superconducting transformation occurs.
Comparative example 3
A method of MoNb film comprising the steps of:
(1) And (3) polishing the surface of the MoNb target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried MoNb target material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2): putting a baffle plate into the sputtering device, closing the cavity, and sequentially opening a cooling water system, a main power supply, a mechanical pump power supply and a machineThe mechanical pump valve and the vacuum indicator are closed when the vacuum degree is lower than 5Pa, the isolation electromagnetic valve, the molecular pump power supply and the molecular pump valve are opened, and the vacuum is pumped until the vacuum degree is better than 8 multiplied by 10 -4 And when Pa, closing the vacuum gauge, and introducing argon gas, wherein the gas flow is controlled to be 60sccm. And after the pressure of the cavity is controlled to be 3Pa, a direct-current power supply is turned on, the power is adjusted to be 15W for starting, and after the glow is stable, the working pressure of the molecular pump valve is adjusted to be kept at 1Pa, and the pre-sputtering is carried out on a sample table without a substrate for 30min.
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 1h, turning off a direct current power supply, and ending sputtering to obtain the Mo80Nb20 film.
The technical effects are as follows:
1. and (3) characterizing the surface morphology of the Mo80Nb20 film prepared in the step (3) through SEM, wherein the film surface is compact and uniform and has no obvious holes.
2. The cross-sectional morphology of the Mo80Nb20 film prepared in the step (3) is characterized by SEM, and the thickness of the film is measured to be 130nm.
3. The structure of the Mo80Nb20 film prepared in the step (3) is characterized by XRD, and no obvious sharp strong peak exists, so that the prepared film is mostly amorphous.
4. And (3) measuring the low-temperature resistance of the Mo80Nb20 film prepared in the step (3) by PPMS, wherein no superconducting transformation occurs.
Comparative example 4
A method of MoNb film comprising the steps of:
(1) And (3) polishing the surface of the MoNb target material by using an electric brush, removing a surface oxide film, sequentially and respectively ultrasonically cleaning by using acetone and absolute ethyl alcohol for 10min, and fixing the dried MoNb target material on a magnetron sputtering target head. And sequentially and respectively ultrasonically cleaning the substrate Si (100) for 10min by using acetone, absolute ethyl alcohol and deionized water, and adhering the substrate Si (100) on a sample plate by using a high-temperature adhesive tape after drying.
(2): putting a baffle plate into the sputtering device, closing the cavity, and sequentially opening a cooling water system, a main power supply and a machineMechanical pump power supply, mechanical pump valve and vacuum indicator, when the vacuum degree is lower than 5Pa, closing the mechanical pump valve, opening the isolation electromagnetic valve, molecular pump power supply and molecular pump valve, and vacuumizing until the vacuum degree is better than 8×10 -4 And when Pa, closing the vacuum gauge, and introducing argon gas, wherein the gas flow is controlled to be 60sccm. And after the pressure of the cavity is controlled to be 3Pa, a direct-current power supply is turned on, the power is adjusted to be 100W for starting, after the glow is stable, the working pressure of the molecular pump valve is adjusted to be kept at 1Pa, and the pre-sputtering is carried out on a sample table without a substrate for 30min.
(3) And after the pre-sputtering time is over, controlling the sample stage to rotate through software, enabling the target to be aligned with the sample stage with the substrate, timing at the same time to serve as sputtering starting time, and after 1h, turning off a direct current power supply, and ending sputtering to obtain the Mo80Nb20 film.
The technical effects are as follows:
1. the Mo80Nb20 film prepared in step (3) was characterized by SEM for its surface morphology, as shown in part (a) of fig. 3, the film surface was dense, uniform, and no significant holes were observed.
2. The Mo80Nb20 thin film prepared in step (3) was characterized in its cross-sectional morphology by SEM, as shown in part (b) of fig. 3, and its thickness was measured to be 1104nm.
3. And (3) representing the structure of the Mo80Nb20 film prepared in the step (3) by XRD, wherein a sharp strong peak is obvious, which indicates that the prepared film is crystallized.
4. And (3) measuring the low-temperature resistance of the Mo80Nb20 film prepared in the step (3) by PPMS, wherein no superconducting transformation occurs.
Examples 1-6 all exhibited superconductive transition phenomena and had higher Tc compared to comparative examples 1-4, indicating that the preparation power could affect the occurrence of superconductive transition phenomena, while the film thickness affected the Tc. Experimental results show that when the sputtering power is lower than 60W, the prepared film is amorphous, and the films prepared at the powers of 60W and 30W can generate superconducting transformation at low temperature. And at sputtering powers above 60W, the films produced are not amorphous and no superconducting transition occurs.
The foregoing is merely a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions easily conceivable by those skilled in the art within the technical scope of the present application should be covered in the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (9)
1. The method for preparing the nano-scale amorphous superconducting film by utilizing the magnetron sputtering is characterized by comprising the following steps of:
sputtering for 10min-3h with sputtering power of 30-60W in an argon environment by utilizing magnetron sputtering, and depositing a target MoNb on a Si substrate to obtain the nanoscale amorphous superconducting film;
the target MoNb is target Mo80Nb20, the purity is higher than 99.95%, and the substrate is Si (100).
2. The method for preparing a nano-scale amorphous superconducting thin film by using magnetron sputtering according to claim 1, wherein the method further comprises target pretreatment and substrate pretreatment before the magnetron sputtering.
3. The method for preparing a nano-scale amorphous superconducting thin film by magnetron sputtering according to claim 2, wherein the target pretreatment comprises the steps of:
polishing the oxide layer on the surface of the target, placing the target in absolute ethyl alcohol and deionized water, performing ultrasonic cleaning, and drying.
4. A method for preparing a nano-scale amorphous superconducting thin film using magnetron sputtering according to claim 2, wherein the substrate pretreatment comprises the steps of:
and ultrasonically cleaning the substrate in absolute ethyl alcohol and deionized water, and then drying.
5. The method for preparing a nano-scale amorphous superconducting thin film according to claim 1, wherein,the vacuum conditions were: firstly, using a mechanical pump to vacuumize until the pressure is below 5Pa, and then using a molecular pump to vacuumize until the pressure is below 8 multiplied by 10 -4 Pa。
6. The method for preparing a nano-scale amorphous superconducting thin film according to claim 1 or 5, wherein the vacuum degree during the sputtering is less than 8 x 10 -4 And after Pa, introducing argon, keeping the flow of the argon gas at 55-65sccm, and keeping the working air pressure at 0.5Pa-1.2Pa by adjusting a molecular pump valve, wherein the temperature is room temperature.
7. The method for preparing a nano-scale amorphous superconducting thin film by magnetron sputtering according to claim 1, wherein the pre-sputtering further comprises pre-sputtering, and the pre-sputtering time is 30min.
8. A nanoscale amorphous superconducting film produced by the method for producing a nanoscale amorphous superconducting film by magnetron sputtering as claimed in any one of claims 1 to 5 and 7.
9. The nano-scale amorphous superconducting film according to claim 8, wherein the nano-scale superconducting film has an amorphous structure and a thickness of 30-900nm;
the nano-scale superconducting film has a superconducting transition phenomenon at a low temperature, and the superconducting transition temperature is 4.4-5.9K.
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