CN108677145A - Method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization - Google Patents

Method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization Download PDF

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CN108677145A
CN108677145A CN201810344717.6A CN201810344717A CN108677145A CN 108677145 A CN108677145 A CN 108677145A CN 201810344717 A CN201810344717 A CN 201810344717A CN 108677145 A CN108677145 A CN 108677145A
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superconducting
epitaxial growth
thin film
metal oxide
element metal
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蔡传兵
曲兰雪
鲁玉明
白传易
郭艳群
刘志勇
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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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
    • C23C14/24—Vacuum evaporation
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
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    • C—CHEMISTRY; METALLURGY
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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
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
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    • 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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    • 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
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Abstract

The present invention provides a kind of methods prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, according to progress initial component vapor deposition the characteristics of metal targets；The nano particle being evaporated by target under high vacuum state is deposited into amorphous metal precursor thin film after reaching substrate, and after deposition, precursor film is transported to the low pressure atmosphere of different partial, then is subject to different temperature and carries out crystallization and epitaxial growth.The method of the present invention realizes the multi-metal element coevaporation of different melting points and sublimation temperature, and the evaporation technique and condition of the element can be chosen according to the characteristics of component, and dynamic baseband can realize the uniformity of forerunner's component；Later stage oxidation processes start from very refined, nano level forerunner's component, and it is more that later stage crystallization grows nuclearing centre, fast growing and density is relatively high；In addition, by controlling partial pressure of oxygen, it can realize and carry out reaction heat treatment at a lower temperature, you can realize that crystallization and epitaxial growth, preparation method are simple at a lower temperature.

Description

Method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization
Technical field
The present invention relates to a kind of preparation method of superconductor, the side prepared more particularly to a kind of superconducting tape serialization Method is applied to high temperature superconducting materia preparing technical field.
Background technology
Multi-element metal oxide film, including high-temperature superconductor (rare earth elements such as REBaCuO, RE=RE=Y, Gd, Dy), Pang Big giant magnetoresistance (LaSrMnO), piezoelectric ceramics (PZT), ferroelectric material etc. have many functional and are widely applied.Such as have Have and is based on ReBa1Cu2O7-δThe second-generation high-temperature superconductor of (REBaCuO) high-temperature superconductor, the knot of this novel electric power material Structure includes metal base band, oxide buffer layer, copper-based oxide, REBaCuO superconducting layers and coat of metal.Second generation high temperature Superconducting tape refers to the terres rares barium-copper oxide superconducting coating conductor based on REBCO-123 series superconducting materials.It is by metal The compositions such as alloy base band, seed layer, barrier layer, cap layer, rare earth barium copper oxide superconducting layer, protective layer and stabilized zone.With first It is compared for Bi based high-temperature superconductive strips, second-generation high-temperature superconductor has higher irreversibility field, higher suiperconducting transition temperature Degree and higher critical current density, can apply at higher temperature and magnetic field, be that various countries high-temperature superconductor field is researched and developed Focus.
Multi-element metal oxide epitaxial film is the basic material of various devices application, these materials contain various metals member Element, in film preparation in the presence of the difficulty for being difficult to customer service, the i.e. fusing point of different metal element and the difference of sublimation temperature and feature. In addition to this, the single technology of preparing often returned often exist component structure is uneven, elements diffusion is serious, surface roughness is big, The defects of hole, secondary phase, especially multilayer coated rear structure are easy to deteriorate, and crystal orientation declines, and crystal orientation and cause Phenomena such as close property is not high is also susceptible to, so there are the situations that multiple technologies route coexists on preparation method.In order to be promoted Large area, the film preparation efficiency of long scale and performance, need to be improved, the technology for becoming urgently to be resolved hurrily is asked using innovative technology Topic.
Invention content
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind Method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, mainly solves the component structure of generally existing Uneven, the defects of elements diffusion is serious, surface roughness is big, hole, secondary phase, is, it can be achieved that different melting points and sublimation temperature Multi-metal element co-evaporates, and the evaporation technique and condition of the element can be chosen according to the characteristics of component, dynamic baseband can Realize that the uniformity of pioneer's component, later stage oxidation processes start from very refined, nano level forerunner's component, the growth of later stage crystallization Nuclearing centre is more, fast growing and density is relatively high, in addition, by controlling partial pressure of oxygen, it can be achieved that carrying out at a lower temperature anti- It should be heat-treated, you can realize crystallization and epitaxial growth at a lower temperature, especially overcome multilayer coated rear structure and be easy to dislike Change, the technical problems such as crystal orientation decline.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, which is characterized in that adopt It is completed, is included the following steps with the two-step method of superconducting tape precursor film deposition process and superconducting phase transition process：
A. in superconducting tape precursor film deposition process, using the preparation method of reaction coevaporation, it is total to carry out multi-element metal Deposition in deposition process, is controlled the mode of movement of strip material substrate, is carried out band using different metal targets as evaporation source Dynamic deposition REBCO films, to prepare superconducting tape precursor film in strip material substrate, wherein RE is rare earth element；
B. in superconducting phase transition process, the strip material substrate of superconducting tape forerunner's film preparation will be completed in the step a It is sent into oxidation reaction apparatus and is heat-treated, the different sections in oxidation reaction apparatus each lead into the oxygen of different flow Gas makes to form different partial pressure of oxygen environment in the different section chambers in oxidation reaction apparatus, to obtain different partial Low pressure atmosphere, and the different sections in oxidation reaction apparatus apply different temperature, super to what is formed in strip material substrate Conduction band material precursor film carries out Crystallizing treatment, realizes the epitaxial growth of superconduction phase transition, to obtain polynary gold in strip material substrate Belong to oxide epitaxial film.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, carrying out instead When should co-evaporate, different metal targets are respectively placed in crucible, according to the fusing point of the metallic element of different metal target and Sublimation temperature is different, using in electron gun, thermal evaporation and ion beam evaporation method any one vacuum film preparation method or The composite vacuum method for manufacturing thin film of the arbitrary several method of person carries out initial component vapor deposition；Under vacuum conditions, by metallic target The nano particle that material is evaporated is deposited into amorphous metal precursor thin film after reaching substrate；It was deposited in superconducting tape precursor film Cheng Zhong makes substrate remain a constant speed movement, to ensure that deposited metal element is uniformly distributed.
It is maintained at eventually in the step a superconducting tapes precursor film deposition process as currently preferred technical solution Not higher than 10-5It is carried out under the high vacuum condition of Torr.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, band is served as a contrast Implement cooling in bottom.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, using volume pair The mode of movement for furling the strip material substrate put makes strip material substrate that by pre-deposition region, it is heavy at the uniform velocity to carry out superconducting tape precursor film Product；And in the step b superconducting phase transition processes, dynamic baseband is made to synchronize the thermal processing chamber by oxidation reaction apparatus, Superconducting phase transition process is completed, realizes that long-range prepares multi-element metal oxide epitaxial film.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, in evaporation cavity The deposition region of top is using the two-way multiply control of band, and band transporting system is to strap tension size, tape transport distance and tape running speed It is set, to realize the long strip deposits of hundred meter levels, realizes the preparation of long-range superconducting tape.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, to binary gold Belong to target, ternary metal target or more multi-element metal target to be co-evaporated, wherein binary metal target is denoted as M respectively1、 M2Or ternary metal target is denoted as M respectively1、M2、M3, or M is denoted as respectively to first metal targets1、M2…Mn, i.e. n >=4, and It is deposited respectively according to gold target material, and deposition rate is monitored in real time, deposition proportioning is controlled by depositing self feed back, Multi-element metal co-deposition is carried out using reaction coevaporation method.
As currently preferred technical solution, in the step b superconducting phase transition processes, oxidation reaction apparatus uses The strip material substrate for completing superconducting tape forerunner's film preparation is sent into oxidation reaction apparatus and is carried out by segmented oxidation reaction tube furnace Fractional Heat-treatment.
As currently preferred technical solution, in the step b superconducting phase transition processes, not higher than 840 DEG C Under lower temperature, reaction heat treatment is carried out to the superconducting tape precursor film prepared on substrate, superconduction can be made at a lower temperature Band precursor film realizes Crystallizing treatment, carries out multi-element metal oxide thin film epitaxial growth.
As currently preferred technical solution, in the step a superconducting tapes precursor film deposition process, including it is as follows Step：
A. start general supply, start compressor, start water cooling unit, so that conduction band material forerunner's film deposition apparatus system is started, open It opens backfill valve backfill nitrogen and opens cavity, using superconducting tape substrate as superconduction base band, after welding superconduction base band and be put into Chamber is rolled up, and after the superconduction base band after welding is transported to pre-deposition region, closes chamber door；
B. start mechanical pump and apparatus for baking, subsequent start-up molecular pump, and after reaching set vacuum degree, close baking Device；
C. using different metal targets as evaporation source, reaction coevaporation equipment, and the pre- thermal evaporation material of thermal evaporation is opened, is seen Examining vapor deposition chamber vacuum has unchanged, after the vacuum of chamber to be deposited is stablized, opens automatic vapor deposition pattern, carries out superconducting tape precursor film Deposition process；While being deposited, superconduction base band transport system is opened, regulates and controls tape running speed and tension, is operated in superconduction Multi-element metal is carried out in base band and is total to Dynamic deposition, to prepare superconducting tape precursor film in superconduction base band.
Include the following steps in the step b superconducting phase transition processes as currently preferred technical solution：
I opens the heating system of oxidation reaction apparatus, and gradient setting is carried out to temperature；
II opens oxygen valve, is set to oxygen flow, and adjust high low oxygen pressure respectively, in oxidation reaction apparatus In different sections be passed through the oxygen of different flow, make to form different oxygen in the different section chambers in oxidation reaction apparatus Divide environment；
III is sent into oxidation instead by superconduction base band transport system, by the strip material substrate for completing superconducting tape forerunner's film preparation It answers and carries out Fractional Heat-treatment in device, multi-element metal oxide epitaxial film is obtained in strip material substrate, turn completing superconducting phase After change process, band is transported to winding chamber and is wound.
As currently preferred technical solution, in the step b superconducting phase transition processes, to oxidation reaction apparatus After the different oxygen pressure of the default height of different sections, the chamber that precursor film passes through oxidation reaction apparatus is made to carry out Crystallizing treatment, superconduction Band after hypoxemia pressure area reacts and to form the secondary phase of oxide and complexity, is then rapidly transformed into hyperoxia pressure area first Superconducting phase obtains multi-element metal oxide epitaxial film to realize superconduction phase transition in strip material substrate.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. component structure that the method for the present invention mainly solves generally existing is uneven, elements diffusion is serious, surface roughness Greatly, the defects of hole, secondary phase, the technical problems such as especially multilayer coated rear structure is easy to deteriorate, and crystal orientation declines；To gold Belong to target controlled respectively, precursor film Dynamic deposition ensure Elemental redistribution uniformly and can realize at a lower temperature crystallization and Epitaxial growth, to realize that quick long-range prepares the purpose of high quality epitaxial film；
2. being deposited into after the nano particle arrival substrate that the present invention under high vacuum state, is evaporated by a variety of targets non- Amorphous metal precursor thin film, substrate remain a constant speed movement to ensure that deposition of elements is uniformly distributed in deposition process；
3. the method for the present invention by control partial pressure of oxygen, it can be achieved that carrying out reaction heat treatment at a lower temperature, you can compared with Crystallization and epitaxial growth are realized under low temperature；
4. the method for the present invention can realize the multi-metal element coevaporation of different melting points and sublimation temperature, can be according to group The evaporation technique and condition of the element are chosen at the characteristics of element, and dynamic baseband can realize the uniformity of forerunner's component；Later stage Oxidation processes start from very refined, nano level forerunner's component, and later stage crystallization growth nuclearing centre is more, fast growing and density It is relatively high；In addition, by controlling partial pressure of oxygen, it can be achieved that carrying out reaction heat treatment at a lower temperature, you can at a lower temperature Realize crystallization and epitaxial growth.
Description of the drawings
Fig. 1 is that one dystopy of the embodiment of the present invention co-evaporates instrument overall structure diagram.
Specific implementation mode
Said program is described further below in conjunction with specific examples of the implementation, the preferred embodiment of the present invention is described in detail such as Under：
Embodiment one
In the present embodiment, referring to Fig. 1, a kind of dystopy coevaporation instrument, including unreeling wheel 1, two-way multiply band transporting system 2, low oxygen pressure chamber 3, high oxygen pressure chamber 4, winding wheel 5, electron beam evaporation 6, thermal evaporation 7 and electron beam evaporation 8 are super with second generation high temperature For conduction band material and combine Fig. 1, the method that detailed description dystopy continuously prepares multi-element metal oxide epitaxial film.This process begins It is maintained at 10 eventually-5It is carried out under Torr vacuum conditions.
In the present embodiment, referring to Fig. 1, prepared by a kind of dystopy multi-element metal oxide thin film epitaxial growth and its serialization Method, include the following steps：
Step 1：General supply starts, compressor start, and water cooling unit starts, booting computer, makes conduction band material precursor film deposition dress System startup is set, backfill valve backfill nitrogen is opened and opens cavity, using superconducting tape substrate as superconduction base band, welds superconduction base After band, i.e., by buffer layer LMO/Epi-MgO/IBAD-MgO/Y2O3/Al2O3/ Hastelloy, which is welded on, unreels chamber, by unreeling After strip coil is put to retracting and be delivered to pre-deposition region by wheel 1 and two-way multiply band transporting system 2, chamber door is closed；
Step 2：Start 4 mechanical pumps and apparatus for baking, is first slightly vacuumized with mechanical pump, wait for vacuum to 10-3Torr with Under, it is then taken out using molecular pump essence so that the vacuum degree that chamber is deposited reaches and is maintained at 10-5Torr, this process need 3h, Gao Zhen Sky deposition can avoid the high nano particle oxidation of activity, after reaching set vacuum degree, close apparatus for baking；
Step 3：Electron gun and the pre- thermal evaporation material of thermal evaporation are opened, observation vapor deposition chamber vacuum has unchanged；If vacuum is steady It is fixed, then automatic vapor deposition pattern is opened after half an hour；Using 3 kinds of metal targets as evaporation source, ternary metal is co-evaporated, Wherein M1、M2、M3Nominal group be divided into Gd：Ba：Cu=1：2：3, three kinds of elements use electron gun and thermal evaporation respectively, in Fig. 1 Middle electron beam evaporation 6, thermal evaporation 7, electron beam evaporation 8 are used as pumping and are sputtered；It is shaken using film thickness gauge and quartz crystal Monitor real time monitoring deposition rate can realize deposition self feed back to be precisely controlled deposition proportioning, really realize ternary coevaporation；
Step 4：While being deposited, superconduction base band transport system is opened, regulates and controls tape running speed and tension, operation exists Multi-element metal is carried out in stranded superconductive base band and is total to Dynamic deposition, to prepare superconducting tape precursor film in superconduction base band；To For the hundred meter level strip deposits for subsequently realizing not less than 100 meters of length, achieve the purpose that preparing long-range band provides equipment support；
Step 5：In Fig. 1, shown low oxygen pressure chamber 3 and high oxygen pressure chamber 4 are heat-treatment zone, by two sections of quartz ampoules, 6 thermoelectricity Even summation temperature measurement module forms, and opens diamond heating system, and gradient-heated is carried out to tube furnace using this 6 thermocouples, until Reach 840 DEG C；By opening the heating system of oxidation reaction apparatus, gradient setting is carried out to temperature；
Step 6：Oxygen valve is opened, oxygen is passed through into tube furnace quartz ampoule, height is realized by independent vacuum pump The control of oxygen pressure adjusts high low oxygen pressure, and is set to oxygen flow, and the different sections in oxidation reaction apparatus are passed through not With the oxygen of flow, different partial needed for phase process is provided into for band, stably reaches default oxygen pressure, wherein high oxygen pressure Area's oxygen presses L-PO2For 12Pa, hyperoxia pressure area oxygen presses H-PO2For 52Pa, make to be formed in the different section chambers in tube furnace different Partial pressure of oxygen environment；
Step 7：After stably reaching default oxygen pressure, by superconduction base band transport system, superconducting tape precursor film system will be completed Standby strip material substrate is sent into oxidation reaction apparatus and carries out crystallization and thermal treatment, relatively low at 840 DEG C when carrying out crystallization and thermal treatment At a temperature of reaction heat treatment is carried out to the superconducting tape precursor film that is prepared on substrate, band is first in hypoxemia pressure area L-PO2Reaction It is formed after oxide and the secondary phase of complexity, then in hyperoxia pressure area H-PO2Superconducting phase is rapidly transformed into, in strip material substrate On obtain multi-element metal oxide epitaxial film, to realize superconduction phase transition speed promoted；The present embodiment method crystallization is given birth to Long nuclearing centre is more, fast growing and density is relatively high；The present embodiment realizes the relatively low temperature at 840 DEG C by controlling partial pressure of oxygen Degree is lower to carry out reaction heat treatment, so that superconducting tape precursor film is realized Crystallizing treatment at a lower temperature, carries out multi-element metal oxidation Object thin film epitaxial growth；
Step 8：After the superconducting phase transition process for completing above-mentioned steps 7, band is transported to winding chamber and is wound.
The present embodiment prepares high-temperature superconducting thin film for physics dystopy method and provides a kind of means, i.e. superconducting tape precursor film is heavy Product with superconduction phase transition be divided into two steps completion, and this " dystopy method " be more easy to superconducting thin film object mutually formed rule expansion probe into. Currently, the preparation method of reaction coevaporation is still rarely reported at home, the present embodiment continuously prepares multi-element metal using dystopy The method of oxide epitaxial film, which is independently built, has run First reaction coevaporation equipment, the roll-to-roll polynary gold of Dynamic deposition Belong to sull and polynary co-deposition not only may be implemented, it can also each evaporation source of independent control.The present embodiment is in high vacuum shape It is deposited into amorphous metal precursor thin film, substrate after the substrate for the nano particle arrival water cooling being evaporated by 3 kinds of targets under state Movement is remained a constant speed in deposition process to ensure that deposition of elements is uniformly distributed；In addition to this, it is co-evaporated by roll-to-roll reaction The mode of deposition can also quickly prepare thick film, have many advantages, such as that component is adjustable, deposition rate is fast, at low cost, it is easier to carry out On a large scale, the high-temperature superconducting thin film production of industrialization.The present embodiment can specify superconducting thin film using this unique " two-step method " And its coating conductor nanoscale forerunner component, crystallization temperature modulation under and formed different from block system object phase relation, Texture growing feature.
Metal targets are respectively placed in graphite crucible or tantalum crucible boat by the present embodiment, are total to using ternary metal target Evaporation, and according to the fusing point of metallic element and the difference of sublimation temperature and feature, use electron gun and thermal evaporation composite vacuum Thin film technique carries out initial component vapor deposition；After water cooling substrate being reached under high vacuum state by the nano particle that target is evaporated It is deposited into amorphous metal both precursor film, substrate remains a constant speed movement to ensure that deposition of elements is uniformly distributed in deposition process； After this deposition, precursor film is roll-to-roll to enter oxidation reaction tube furnace, the oxygen of different flow is passed through in tube furnace, to obtain The low pressure atmosphere for obtaining different partial is subject to different temperature and carries out crystallization and epitaxial growth.The present embodiment the method is realized not It is co-evaporated with fusing point and the multi-metal element of sublimation temperature, the present embodiment chooses the steaming of the element according to the characteristics of component Hair technology and condition, dynamic baseband can realize that the uniformity of pioneer's component, later stage oxidation processes start from very refined, nanoscale Forerunner's component, it is more that later stage crystallization grows nuclearing centre, fast growing and density is relatively high, in addition, by controlling partial pressure of oxygen, energy Realization carries out reaction heat treatment at a lower temperature, can realize crystallization and epitaxial growth at a lower temperature.
The present embodiment is completed using superconducting tape precursor film deposition process and the two-step method of superconducting phase transition process；In superconduction In band precursor film deposition process, multi-element metal co-deposition is carried out using the preparation method of reaction coevaporation, with different metals Target is as evaporation source, in deposition process, controls the mode of movement of strip material substrate, carries out band Dynamic deposition film, to Superconducting tape precursor film is prepared in strip material substrate, wherein RE is rare earth element；In superconducting phase transition process, superconduction will be completed The strip material substrate of band forerunner's film preparation is sent into oxidation reaction apparatus and is heat-treated, the not same district in oxidation reaction apparatus Section is passed through the oxygen of different flow, makes to form different partial pressure of oxygen environment in the different section chambers in oxidation reaction apparatus, To obtain the low pressure atmosphere of different partial, the different sections in oxidation reaction apparatus apply different temperature, in band The superconducting tape precursor film formed on material substrate carries out Crystallizing treatment, the epitaxial growth of superconduction phase transition is realized, in strip material substrate On obtain multi-element metal oxide epitaxial film.
The present embodiment use dystopy method, have component is adjustable, deposition rate is fast, it is at low cost, be suitable for the advantages such as industrialization, The present embodiment has prepared the very excellent multi-element metal oxide epitaxial film of performance using dystopy reaction coevaporation technique.Solution The defects of certainly component structure of generally existing is uneven, elements diffusion is serious, surface roughness is big, hole, secondary phase.Especially The technical problems such as structure is easy to deteriorate after multilayer coated, and crystal orientation declines.
The present embodiment is according to progress initial component vapor deposition the characteristics of metal targets；It is evaporated by target under high vacuum state The nano particle come is deposited into amorphous metal precursor thin film after reaching substrate, and after deposition, precursor film is transported to different oxygen The low pressure atmosphere of partial pressure, then be subject to different temperature and carry out crystallization and epitaxial growth.The present embodiment method realize different melting points and The multi-metal element of sublimation temperature co-evaporates, and the evaporation technique and condition of the element can be chosen according to the characteristics of component, And dynamic baseband can realize the uniformity of forerunner's component；Later stage oxidation processes start from very refined, nano level forerunner's component, It is more that later stage crystallization grows nuclearing centre, fast growing and density is relatively high；In addition, by controlling partial pressure of oxygen, can realize relatively low At a temperature of carry out reaction heat treatment, you can at a lower temperature realize crystallization and epitaxial growth, preparation method it is simple.
Embodiment two
The present embodiment and embodiment one are essentially identical, are particular in that：
In the present embodiment, a kind of method that prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, Include the following steps：
This step of step 1. is identical as embodiment one；
This step of step 2. is identical as embodiment one；
This step of step 3. is identical as embodiment one；
Step 4. opens superconduction base band transport system, regulation and control band Tensity size, tape transport distance while being deposited And tape running speed, it being controlled using the two-way multiply of band, operation carries out multi-element metal in stranded superconductive base band and is total to Dynamic deposition, from And superconducting tape precursor film is prepared in superconduction base band；While being deposited, superconduction base band transport system is opened, regulation and control are walked Tape speed and tension, operation carries out multi-element metal in stranded superconductive base band and is total to Dynamic deposition, to be prepared in superconduction base band Superconducting tape precursor film；To be the follow-up hundred meter level strip deposits realized not less than 100 meters of length, reaches and prepare long-range band Purpose provide equipment support；
This step of step 5. is identical as embodiment one；
This step of step 6. is identical as embodiment one；
This step of step 7. is identical as embodiment one；
This step of step 8. is identical as embodiment one.
In the present embodiment, in superconducting tape precursor film deposition process, using roll-to-roll folding and unfolding strip material substrate it is defeated Mode is sent, strip material substrate is made at the uniform velocity by pre-deposition region, to carry out superconducting tape precursor film deposition；And it is logical so that dynamic baseband is synchronized The thermal processing chamber of peroxidization device completes superconducting phase transition process, realizes that long-range prepares multi-element metal oxide extension Film.Deposition region above evaporation cavity using the two-way multiply control of band, band transporting system to strap tension size, tape transport away from From and tape running speed set, to realize the long strip deposits of hundred meter levels, realize long-range superconducting tape preparation.
The present embodiment is in superconducting tape precursor film deposition process, using the conveying side of the strip material substrate of roll-to-roll folding and unfolding Formula makes strip material substrate at the uniform velocity by pre-deposition region, carry out superconducting tape precursor film deposition；And in superconducting phase transition process, So that dynamic baseband is synchronized the thermal processing chamber by oxidation reaction apparatus, complete superconducting phase transition process, it is more to realize prepared by long-range First metal oxide epitaxial film.The present embodiment is according to progress initial component vapor deposition the characteristics of metal targets；In high vacuum state Under the nano particle that is evaporated by target reach substrate after be deposited into amorphous metal precursor thin film, after deposition, forerunner Film is transported to the low pressure atmosphere of different partial, then is subject to different temperature and carries out crystallization and epitaxial growth.The present embodiment method The multi-metal element coevaporation for realizing different melting points and sublimation temperature, can choose the steaming of the element according to the characteristics of component Hair technology and condition, and dynamic baseband can realize the uniformity of forerunner's component；Later stage oxidation processes start from very refined, nanometer Forerunner's component of grade, it is more that later stage crystallization grows nuclearing centre, fast growing and density is relatively high；In addition, by controlling partial pressure of oxygen, It can realize and carry out reaction heat treatment at a lower temperature, you can realize crystallization and epitaxial growth, preparation method at a lower temperature Simply.
Above in conjunction with saying that the embodiment of the present invention is illustrated in attached drawing, but the present invention is not limited to the above embodiments, may be used also A variety of variations, the Spirit Essence and principle of all technical solutions according to the present invention are made with the purpose of innovation and creation according to the present invention Under change, modification, replacement, combination or the simplification made, equivalent substitute mode is should be, as long as meeting the invention mesh of the present invention , without departing from the technology original of method prepared by dystopy multi-element metal oxide thin film epitaxial growth of the present invention and its serialization Reason and inventive concept, belong to protection scope of the present invention.

Claims (12)

1. a kind of method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, which is characterized in that use Superconducting tape precursor film deposition process and the two-step method of superconducting phase transition process are completed, and are included the following steps：
A. in superconducting tape precursor film deposition process, using the preparation method of reaction coevaporation, multi-element metal co-deposition is carried out, Using different metal targets as evaporation source, in deposition process, the mode of movement of strip material substrate is controlled, it is heavy to carry out band dynamic Product REBCO films, to prepare superconducting tape precursor film in strip material substrate, wherein RE is rare earth element；
B. in superconducting phase transition process, the strip material substrate that superconducting tape forerunner's film preparation is completed in the step a is sent into It is heat-treated in oxidation reaction apparatus, the different sections in oxidation reaction apparatus each lead into the oxygen of different flow, make Different partial pressure of oxygen environment is formed in different section chambers in oxidation reaction apparatus, to obtain the low pressure of different partial Atmosphere, and the different sections in oxidation reaction apparatus apply different temperature, to the superconducting tape formed in strip material substrate Precursor film carries out Crystallizing treatment, realizes the epitaxial growth of superconduction phase transition, to obtain multi-element metal oxidation in strip material substrate Object epitaxial film.
2. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, when carrying out reaction coevaporation, by different metals Target is respectively placed in crucible, different according to the fusing point of the metallic element of different metal target and sublimation temperature, using electron gun, The combined type of any one vacuum film preparation method or arbitrary several method in thermal evaporation and ion beam evaporation method is true Empty method for manufacturing thin film carries out initial component vapor deposition；Under vacuum conditions, it is reached by the nano particle that metal targets are evaporated Amorphous metal precursor thin film is deposited into after substrate；In superconducting tape precursor film deposition process, substrate is made to remain a constant speed movement, To ensure that deposited metal element is uniformly distributed.
3. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, it is maintained at eventually not higher than 10-5The high vacuum item of Torr It is carried out under part.
4. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, strip material substrate is implemented to cool down.
5. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, using the conveying side of the strip material substrate of roll-to-roll folding and unfolding Formula makes strip material substrate at the uniform velocity by pre-deposition region, carry out superconducting tape precursor film deposition；And turn in the step b superconducting phases During change, dynamic baseband is made to synchronize the thermal processing chamber by oxidation reaction apparatus, complete superconducting phase transition process, realizes length Journey prepares multi-element metal oxide epitaxial film.
6. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, the deposition region above evaporation cavity is double using band It is controlled to multiply, band transporting system sets strap tension size, tape transport distance and tape running speed, to realize that hundred meter levels are long Strip deposits realize the preparation of long-range superconducting tape.
7. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step a superconducting tapes precursor film deposition process, to binary metal target, ternary metal target or More multi-element metal target is co-evaporated, and wherein binary metal target is denoted as M respectively1、M2Or ternary metal target difference It is denoted as M1、M2、M3, or M is denoted as respectively to first metal targets1、M2…Mn, i.e. n >=4, and deposited respectively according to gold target material, And deposition rate is monitored in real time, deposition proportioning is controlled by depositing self feed back, is carried out using reaction coevaporation method Multi-element metal is co-deposited.
8. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step b superconducting phase transition processes, oxidation reaction apparatus uses segmented oxidation reaction tube furnace, will It completes to carry out Fractional Heat-treatment in the strip material substrate feeding oxidation reaction apparatus of superconducting tape forerunner's film preparation.
9. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that：In the step b superconducting phase transition processes, under the lower temperature not higher than 840 DEG C, to what is prepared on substrate Superconducting tape precursor film carries out reaction heat treatment, and superconducting tape precursor film can be made to realize Crystallizing treatment at a lower temperature, into Row multi-element metal oxide thin film epitaxial growth.
10. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that, in the step a superconducting tapes precursor film deposition process, includes the following steps：
A. start general supply, start compressor, start water cooling unit, so that conduction band material forerunner's film deposition apparatus system is started, open back It fills out valve backfill and nitrogen and opens cavity, using superconducting tape substrate as superconduction base band, after welding superconduction base band and be put into and unreel chamber, And after the superconduction base band after welding is transported to pre-deposition region, chamber door is closed；
B. start mechanical pump and apparatus for baking, subsequent start-up molecular pump, and after reaching set vacuum degree, close baking dress It sets；
C. using different metal targets as evaporation source, reaction coevaporation equipment is opened, and the pre- thermal evaporation material of thermal evaporation, observation are steamed Plating chamber vacuum has unchanged, after the vacuum of chamber to be deposited is stablized, opens automatic vapor deposition pattern, carries out superconducting tape precursor film deposition Process；While being deposited, superconduction base band transport system is opened, regulates and controls tape running speed and tension, is operated in superconduction base band Upper progress multi-element metal is total to Dynamic deposition, to prepare superconducting tape precursor film in superconduction base band.
11. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that, in the step b superconducting phase transition processes, includes the following steps：
I opens the heating system of oxidation reaction apparatus, and gradient setting is carried out to temperature；
II opens oxygen valve, is set to oxygen flow, and adjust high low oxygen pressure respectively, in oxidation reaction apparatus Different sections are passed through the oxygen of different flow, make to form different partials pressure of oxygen in the different section chambers in oxidation reaction apparatus Environment；
III is sent into oxidation reaction dress by superconduction base band transport system, by the strip material substrate for completing superconducting tape forerunner's film preparation Middle carry out Fractional Heat-treatment is set, multi-element metal oxide epitaxial film is obtained in strip material substrate, completes superconduction phase transition mistake Band is transported to winding chamber and wound by Cheng Hou.
12. the method that according to claim 1 prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization, It is characterized in that, in the step b superconducting phase transition processes, the different oxygen of height is preset to the different sections of oxidation reaction apparatus After pressure, the chamber that precursor film passes through oxidation reaction apparatus is set to carry out Crystallizing treatment, superconducting tape reacts shape in hypoxemia pressure area first After oxide and the secondary phase of complexity, superconducting phase then is rapidly transformed into hyperoxia pressure area, to realize that superconducting phase turns Become, multi-element metal oxide epitaxial film is obtained in strip material substrate.
CN201810344717.6A 2018-04-17 2018-04-17 Method prepared by dystopy multi-element metal oxide thin film epitaxial growth and its serialization Pending CN108677145A (en)

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