CN114242335B - Production process for kilometer-level IBAD-MgO long belt - Google Patents
Production process for kilometer-level IBAD-MgO long belt Download PDFInfo
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- CN114242335B CN114242335B CN202111656909.9A CN202111656909A CN114242335B CN 114242335 B CN114242335 B CN 114242335B CN 202111656909 A CN202111656909 A CN 202111656909A CN 114242335 B CN114242335 B CN 114242335B
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 21
- 230000008021 deposition Effects 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000002128 reflection high energy electron diffraction Methods 0.000 claims abstract 6
- 238000000034 method Methods 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 description 6
- 238000007735 ion beam assisted deposition Methods 0.000 description 5
- 238000010884 ion-beam technique Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
- H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
- H01B12/06—Films or wires on bases or cores
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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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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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a production process for a kilometer-level IBAD-MgO long belt, which comprises the following steps: opening RHEED and KSA400 software, selecting a proper acquisition frame, fixing the initial position and width of the acquisition frame, and automatically adjusting the height according to the size of the diffraction spots; adjusting the exposure time of the image so that the highest intensity of the image in the acquisition frame is maintained at about 50%; the software captures n two-dimensional lattice images diffracted by RHEED at certain interval time; extracting data of standard deviation and average intensity from the histogram of each image; calculating the ratio of standard deviation to average intensity by software and calculating the average value of the ratio of n two-dimensional lattice images; the calculated average value is compared with the value of the optimal preparation process condition. The beam current of the deposition source is adjusted within a range of allowable differences. Therefore, the quality of MgO quasi-single crystal growth can be accurately judged, and the range of ion source parameters to be adjusted can be accurately judged.
Description
Technical Field
The invention relates to the technical field of superconducting materials, in particular to a production process for a kilometer-level IBAD-MgO long tape.
Background
The high temperature superconducting material has the characteristics of complete zero resistance and complete diamagnetism at low temperature. The magnetic resistance of the magnetic material has huge application prospect in the fields of industry, national defense, scientific research and medicine, and the development of superconducting technology is very important to the governments of various countries in the world. Compared with the first-generation bismuth-system high-temperature superconducting tape, the second-generation high-temperature superconducting tape has the potential advantages of critical current density higher by two orders of magnitude, excellent current carrying capacity under a magnetic field, high mechanical strength, low cost and the like, so that the second-generation high-temperature superconducting tape becomes the most promising industrialized material.
The coherence length of the high temperature superconducting material is very short, about 7 nm. The larger the grain boundary angle, the larger the non-superconducting transition region of the grain boundary, and the easier the weak connection is formed. The twin experiments show that Ic drops sharply when the grain boundary angle is greater than 4 degrees, so in order to obtain a high Ic that is not limited by weak links, the superconducting thin film must be formed into a highly textured thin film. Through the development of second-generation high-temperature superconducting tapes, the IBAD (ion beam assisted deposition) technology capable of preparing low-cost quasi-monocrystalline films on any substrate is developed first in the United states of America, and is also a main method for forming a texture layer on a non-monocrystalline substrate in the industry at present.
The method for preparing the textured layer film of the high-temperature superconductive tape currently adopts an IBAD (ion beam assisted deposition) method generally internationally, and adopts a form of evaporation coating only by adopting different sources, and adopts a radio frequency sputtering coating form according to the following principle: the deposition source bombards the magnesium target with ion beams emitted by a divergent angle under high vacuum, the bombarded magnesium target component reacts with oxygen in a molecular or atomic form on the arc plate to form MgO, the auxiliary source bombards MgO deposited on the strip material with the ion beams emitted by an angle parallel to the ion grid mesh, the unnecessary grain surface is bombarded, only the MgO (100) surface is reserved to achieve the aim of orderly arranging grains, and the deposition film and the bombarded strip material are synchronously carried out. We have now used RHEED (high energy electron diffractometer) and equipped with KSA400 analysis software to monitor the whole preparation process of long bands in situ (shown in FIG. 5) to monitor MgO surface morphology and quasi-single crystal growth in real time by means of the diffracted speckle images. Because the thickness of MgO prepared by IBAD is only about 10nm, and the MgO cannot be directly used and measured, the MgO must be subjected to epitaxial MgO thickening treatment, and then epitaxial LMO preparation is carried out on the surface of the epitaxial MgO, so that a proper surface is provided for the subsequent YBCO superconductive layer (shown in figure 6). For the kilometer-level IBAD-MgO long belt preparation process, the required traction belt speed is about 3-4m/min, the whole preparation process can be completed in five or six hours, and in the production process, the deposition rate gradually decreases along with the cleanliness of the target surface, the environment of the chamber is poorer and worse, so that the initial process parameter condition cannot meet the kilometer-level belt production, and how to adjust the power supply parameters of the ion source in the long belt process preparation process is very important.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a production process for a kilometer-level IBAD-MgO long belt, which can accurately judge the quality of crystal growth, accurately judge the range of ion source parameters to be adjusted, and obtain a stable kilometer-level superconducting belt texture layer preparation process by accurately adjusting the ion source parameters.
The technical scheme of the invention is as follows:
the invention aims to provide a production process for a kilometer-grade IBAD-MgO long belt, which comprises the following steps of:
opening the RHEED high-energy electron diffractometer and matched KSA400 software, selecting a proper acquisition frame, fixing the initial position and width of the acquisition frame, and adjusting the height according to diffraction spots;
adjusting the exposure time of the image so that the highest intensity of the image in the acquisition frame is maintained at about 50%;
after confirming the proper position, the software captures n (n is a natural number greater than or equal to 2) two-dimensional lattice images diffracted by RHEED at certain interval time;
extracting Std detection and Average Intensity data from the histogram of each two-dimensional lattice image;
calculating the ratio of Std devition to Average Intensity by software and calculating the average value of the ratio of n two-dimensional lattice images;
comparing the calculated average value with the numerical value of the optimal preparation process condition, and adjusting the beam current of the deposition source within the allowable difference range.
Preferably, the height is adjusted according to the diffraction spot from the step of adjusting, the acquisition frame is required to cover the diffraction spot with an intensity of not more than 50% in the second layer displayed in the software.
Preferably, in the step of capturing n two-dimensional lattice images diffracted by RHEED, the interval is 0.1s.
Preferably, in the step of capturing n two-dimensional lattice images diffracted by RHEED, n has a value of 10.
Preferably, the allowable difference range is ±0.15, and if the compared value is higher than the allowable difference range, the beam current of the deposition source is reduced; otherwise, the beam current of the deposition source is increased.
Preferably, the step of adjusting the beam current of the deposition source within the allowable difference further includes cycling and the time of one cycle period is 7min.
Compared with the prior art, the invention has the advantages that:
the production process for the kilometer-level IBAD-MgO long belt can accurately judge the quality of crystal growth, accurately judge the range of ion source parameters to be adjusted, and obtain a stable kilometer-level superconducting belt texture layer preparation process by accurately adjusting the ion source parameters.
Drawings
The invention is further described below with reference to the accompanying drawings and examples:
FIG. 1 is a flow chart of a production process for kilometer grade IBAD-MgO long tapes according to an embodiment of the present invention;
FIG. 2 is an LMO out-of-plane texture of an isolation layer of a kilometer length superconducting tape prepared by a kilometer-sized IBAD-MgO long tape production process according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a collection frame for use in a kilometer class IBAD-MgO long tape production process according to an embodiment of the present invention;
FIG. 4 is a graph showing the variation of the current of a deposition source ion beam in a production process for kilometer-scale IBAD-MgO long tapes according to an embodiment of the present invention;
FIG. 5 is a block diagram of the present invention in the background of the invention for in-situ monitoring of the entire manufacturing process of a long ribbon using an analysis software using a RHEED (high energy electron diffractometer) and equipped with KSA 400;
FIG. 6 is a schematic diagram of the structure of epitaxial LMO preparation on the surface of epitaxial MgO in the background of the invention.
Detailed Description
The objects, technical solutions and advantages of the present invention will become more apparent by the following detailed description of the present invention with reference to the accompanying drawings. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Examples:
referring to fig. 1 to 4, a process for producing a kilometer class IBAD-MgO long tape according to an embodiment of the present invention includes the steps of:
opening the software of the RHEED high-energy electron diffractometer and the KSA400, selecting a proper acquisition frame, fixing the initial position and the width of the acquisition frame, and adjusting the height according to diffraction spots;
adjusting the exposure time of the image so that the highest intensity of the image in the acquisition frame is maintained at about 50%;
after confirming the proper position, the software captures n (n is a natural number greater than or equal to 2) two-dimensional lattice images diffracted by RHEED at certain interval time;
extracting Std device (standard Deviation) and Average Intensity (average intensity) data from the histogram of each two-dimensional lattice image;
calculating the ratio of Std devition to Average Intensity by software and calculating the average value of the ratio of n two-dimensional lattice images;
comparing the calculated average value with the numerical value of the optimal preparation process condition, and adjusting the beam current of the deposition source within the allowable difference range. Specifically, when the calculated average value is lower than the optimal process value, mgO is in an auxiliary source oversupplied state, and the beam current of the deposition source needs to be increased; above the optimal process value, mgO is in the under-bombarded state of the auxiliary source, and the beam current of the deposition source needs to be reduced.
According to the embodiment of the invention, the average value of the ratio of the two-dimensional lattice image is calculated through software, and compared with the numerical value of the optimal preparation process condition, the range of the ion source parameter to be adjusted can be accurately judged, the problem that the adjustment range cannot be accurately judged due to the fact that the ion source parameter is adjusted only through the image in the prior art is solved, and the stable kilometer-level superconducting strip texture layer preparation process is obtained through accurately adjusting the ion source parameter. As shown in fig. 2, it can be seen from the graph that the FWHM of the kilometer-sized strip, that is, the full width at half maximum, fluctuation range of degrees is maintained within the range of 0.2 degrees, that is, the texture of the strip is at a stable value, the growth process of the strip is reasonable, and the texture layer of the kilometer-sized superconducting strip can be stably produced.
In particular, in the step of adjusting the height according to the diffraction spots, the acquisition frame needs to cover three diffraction spots with an intensity of not more than 50% in the second layer displayed in the software. More specifically, the width of the acquisition frame, i.e. the length of the acquisition frame as in fig. 3, is fixed, the initial position of the acquisition frame, i.e. the left end position of the acquisition frame as in fig. 3, is also fixed, and the height of the acquisition frame, i.e. the height of the acquisition frame as in fig. 3, is adjusted according to the size of the diffraction spots.
In the embodiment of the invention, preferably, 10 two-dimensional lattice images diffracted by a RHEED (high-energy electron diffractometer) are captured at intervals of 0.1s, and optionally, other intervals such as 0.05s, 0.15s and the like can be adopted, and the number of captured images can be other numbers such as 20 and the like.
According to the embodiment of the invention, std detection and Average Intensity (average intensity) data are extracted from the histogram of each two-dimensional lattice image; the ratio of Std devitation to Average Intensity is calculated through software, and the average value of the ratio of n two-dimensional lattice images is calculated, so that the crystal growth condition of MgO can be accurately judged in a certain range, and the defect that in the prior art, the growth condition of MgO crystals is judged by only observing RHEED diffraction spot images and staff is required to accumulate and judge according to experience is overcome. By adopting the method of the embodiment of the invention, when the average value is lower than the optimal process value, mgO is in the state of over-bombardment of the auxiliary source, and the beam current of the deposition source needs to be increased. If the average value is higher than the optimal process value, mgO is in the underbombarded state of the auxiliary source, and the beam current of the deposition source needs to be reduced. In the existing production process, the reason that the crystal production is poor due to the fact that the ion beam of the auxiliary source in the RHEED image flows through the large or the small can not be judged, namely the reason that the ion beam is over-bombarded or under-bombarded can be judged.
In the embodiment of the invention, the allowable difference range is +/-0.15, and if the compared value is higher than the allowable difference range, the beam current of the deposition source is reduced; otherwise, the beam current of the deposition source is increased.
In the embodiment of the present invention, as shown in fig. 4, after the step of adjusting the beam current of the deposition source within the allowable difference range, the method further includes a cycle and the time of one cycle period is 7min, that is, the two-dimensional lattice images diffracted by n RHEED are snap-shot every 7min, that is, the certain interval time in the snap-shot step is 7min. Alternatively, the time of the cycle may be other time, which is not specifically described in detail and is determined according to the pulling speed of the tape and the size of the apparatus.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explanation of the principles of the present invention and are in no way limiting of the invention. Accordingly, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention. Furthermore, the appended claims are intended to cover all such changes and modifications that fall within the scope and boundary of the appended claims, or equivalents of such scope and boundary.
Claims (6)
1. A production process for kilometer-grade IBAD-MgO long tapes, comprising the steps of:
opening the software of the RHEED high-energy electron diffractometer and the KSA400, selecting a proper acquisition frame on the image, wherein the initial position and the length of the acquisition frame are generally fixed, and the height is automatically adjusted according to the actual diffraction spot size;
adjusting the exposure time of the image so that the highest intensity of the image in the acquisition frame is maintained at about 50%;
after confirming the proper position, the software captures n two-dimensional lattice images diffracted by RHEED at certain interval time, wherein n is a natural number greater than or equal to 2;
extracting Std detection and Average Intensity data from the histogram of each two-dimensional lattice image;
calculating the ratio of Std devition to Average Intensity by software and calculating the average value of the ratio of n two-dimensional lattice images;
comparing the calculated average value with the numerical value of the optimal preparation process condition, and adjusting the beam current of the deposition source within the allowable difference range.
2. The process for producing a kilometer-scale IBAD-MgO long tape according to claim 1, wherein the step of self-adjusting the height according to the actual diffraction spots, the acquisition frame is required to cover the diffraction spots in the second layer displayed in the software with an intensity of not more than 50%.
3. The process for producing a kilometer-scale IBAD-MgO long tape according to claim 1, wherein the step of snap-photographing n RHEED diffraction two-dimensional lattice images is performed at a spacing of 0.1s.
4. A process for producing a kilometer-scale IBAD-MgO long tape according to claim 1 or 3, wherein in the step of snap-photographing n RHEED diffracted two-dimensional lattice images, the value of n is 10.
5. The process for producing a kilometer class IBAD-MgO long tape according to claim 1, wherein the allowable difference range is ± 0.15, and if the compared value is higher than the allowable difference range, the beam current of the deposition source is reduced; otherwise, the beam current of the deposition source is increased.
6. The process for producing a kilometer-scale IBAD-MgO long tape according to claim 1, further comprising a cycle after the step of adjusting the beam current of the deposition source within an allowable difference range and a cycle time of 7min.
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| US6899928B1 (en) * | 2002-07-29 | 2005-05-31 | The Regents Of The University Of California | Dual ion beam assisted deposition of biaxially textured template layers |
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| US20210148004A1 (en) * | 2017-06-13 | 2021-05-20 | Board Of Trustees Of Michigan State University | Method for fabricating epitaxial halide perovskite films and devices |
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