CN100336237C - Method for modifying ion surface for making high-temperature superconductive device - Google Patents
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Abstract
The present invention relates to a method for modifying ion surface for manufacturing high-temperature superconductive devices. The method uses an ion bombardment mode which can be a sputtering mode or an ion implantation mode. The angle and the distance between an ion source and a bombarded material are properly selected to enhance the evenness of ion beam sputtering, and a certain included angle can be formed between the incidence direction of an ion beam and a normal line on the surface of a sputtered material. Suitable ion energy and scan mode are used for preventing remainder generated by ion bombardment from filling into the valley bottom of a film; noble gas, or reaction gas or the mixed gas of the noble gas and the reaction gas can be used as the ion source, and the cross section pattern of a proper ion beam can be selected. With simple steps and easy operation, the method of the present invention can strengthen the flatness and the organization structure of a surface under processing, reduce surface defects and enhance the superconductive performance of a whole device.
Description
Technical field
The present invention relates to the manufacture method of superconductive device, what be specifically related to is a kind of method for modifying ion surface of making high-temperature superconductive device, utilize this method can strengthen the evenness and the texture of surface to be machined, reduce blemish, thereby finally improve the superconductivity of device.
Background technology
High-temperature superconductive device development has obtained the achievement that attracts people's attention so far, but still exists some problems, particularly the still difficult requirement of satisfying industrial applications aspect the evenness of material surface and texture.Normally a kind of sandwich construction of high-temperature superconducting thin film in the high-temperature superconductive device is comprising substrate, intermediate layer (barrier layer) and high temperature superconducting film itself.Influence high-temperature superconducting thin film superconductivity at first be the quality of superconducting film itself, evenness, orientation, defect distribution and grain boundary properties comprising film, and along with the increase of the thickness of film, the surface quality of superconducting film is easy to worsen, thereby influences the growth of subsequent film; Next is the quality on substrate and barrier layer, because high temperature superconducting film itself does not generally have texture, its texture is to form by substrate and barrier layer " transmission ", so improve the evenness on superconducting film itself, substrate and barrier layer and the superconductivity that texture helps improving whole high-temperature superconducting thin film.On the other hand, some high-temperature superconductive device is first material compression moulding, sintering, growth at high temperature then, and the surface of its final products is usually more coarse, also may have defectives such as hole, space and crackle, thereby reduce its superconductivity.Therefore, the evenness on control material surface and institutional framework have very crucial effect to making high-quality high-temperature superconductive device in the process of preparation high-temperature superconductive device.
At present, the technology of preparation high temperature superconducting materia has a lot, and mainly be divided into two big classes: a class is a vacuum technology, and another kind of is adopting non-vacuum process.As prepare and ion beam assisted depositing method (IBAD), rolling auxiliary biaxial texture method (RABiTS) arranged the vacuum method of high-temperature superconductor film conductor, modify polarization splash method (MBS), inclined substrate sedimentation (ISD), pulsed laser deposition (PLD), sputtering method, electron beam evaporating method (E-beam evaporation) and chemical vapour deposition technique (CVD), comprising Metalorganic Chemical Vapor Deposition (MOCVD); The antivacuum method of preparation high-temperature superconductor film conductor generally comprises sol-gal process (sol-gel), aerosol/spray heating decomposition (Aerosols/spray pyrolysis), deposition of metal organic method (MOD), electrophoresis (electrophoresis), liquid phase epitaxial method and silk screen print method etc.
The advantage of vacuum method is that material has evenness and texture preferably, and defective is few, the critical current density jc height, its shortcoming is to need higher temperature and long reaction time, cause production cost higher, production efficiency is lower, so just is difficult to realize large-scale industrial production.
At present, adopt antivacuum method to prepare high temperature superconducting materia mostly.The characteristics of adopting non-vacuum process are easy operations, with short production cycle, with low cost, can fairly largely produce.
Briefly introduce several antivacuum methods below:
(1) sol-gel process
US6,235,402 grades propose sol-gel process, and it is to adopt to dip coating processes and make the solution that has dissolved pre-powder process form film, dries then and heat treatment, and its typical technological process is as follows:
The dissolving of the 1. preparation of sol---pioneer's masterbatch (being generally nitrate, alkoxide, acetate etc.);
2. the preparation of gel---evaporating liquid is removed most of solvent, and dissolving forms gel again;
3. dip-coating (dip coating) or spin coating (spin coating);
4. heating and decomposition, oxidation are to form required film.
Sol gel process is with low cost, rapidly and efficiently, and impurity content is few, composition is even, preparation temperature is low, can be fit to large-scale production, is a kind of simple preparation technology.But easily produce deposition in the gel heat treatment process, the prepared film surface is more coarse, exists hole, crackle and second to equate defective.Utilize the loaded current of the high temperature superconducting film of this method preparation can't satisfy industrial application requirements at present.
(2) aerosol/spray heating decomposition
US6,261,704 propose aerosol/spray heating decomposition, the basic technology of this method is to be dissolved in cuprate class (being generally nitrate, alkoxide, acetate etc.) in the aqueous solution of nitric acid in proportion earlier, then it is made aerosol, with this aerosol spray (substrates such as Ni, Al, Cu) to the substrate that is heated to uniform temperature, the sample after the spraying is put into distinguishes molten the processing in the zone melting furnace, carry out sintering at last under particular atmosphere with sprayer unit.
This method needs special sprayer unit, make its cost than other adopting non-vacuum process height, and the prepared film surface is generally more coarse, has defective in the film.Utilize the prepared high-temperature superconducting thin film of this method also to be difficult to practicability at present.
(3) deposition of metal organic method
Deposition of metal organic technology [1] is a kind of method that forms homogeneous film from liquid solution.The general technology flow process is for to be dissolved in the stoichiometric proportion of acetate compound according to strictness in pioneer's masterbatch, then this solution is dissolved in the organic solvent, the solution for preparing by dip-coating or spin-on deposition on smooth substrate surface, last drying at high temperature, oxygenation are handled and are obtained required material.This technology is generally with SrTiO
3, LaAlO
3Or sapphire single-crystal is a backing material.
This method has short, the low cost and other advantages of deposition process, and is easy to control the end product composition, can be on irregular substrate the shape film, be suitable for large-scale production.But, utilize the MOD method to be difficult to make the required thick film of industry, easily produce deposit, the film surface of preparation is more coarse usually, has defective in the film.
(4) electrophoretic deposition
This method [2] is to adopt electrochemical method, and the charged pre-powder process that utilizes electric field will be suspended in the solution is deposited on substrate surface.Its general technology flow process is: pre-powder process is dissolved in makes suspended substance in the acetone, the aluminium oxide flat board that will cover silver is then done cathode substrate, stainless steel cloth is dipped in makes anode in the suspended substance, in suspended substance, put into additive and add that certain electrode voltage carries out overlay film.
This method has deposition rate height, simple operation and other advantages, but the microstructure of prepared film is relatively poor, and the surface is more coarse, have defective in the film, density is very low, and its composition is wayward, make that the critical current density that is reached is lower, be difficult to satisfy the commercial Application requirement.
(5) liquid phase epitaxial method
US6,008,162 proposes liquid phase epitaxial method, promptly at high temperature adopts top seed crystal melt growth method to prepare well behaved superconducting film the BaO-CuO molten oxide.
This method can form film under normal pressure, and the stoichiometric proportion of film accurately, fast growth, degree of crystallinity height.The shortcoming of this method is that the general microstructure of prepared film is relatively poor, the surface is more coarse, there are defective and large angle boundary in the film, and, need higher working temperature, not only increased cost, and between solution and backing material, be easy to produce chemical reaction, made the decreased performance of material.
(6) silk screen printing
This method [3] is that pre-powder process and suitable adhesive (as polyvinyl alcohol) are fully mixed, be equipped with solvent, make slurries with certain flowability, make its mesh screen that passes through given shape and brush a certain specific region at substrate (as ZrO2, Al2O3, MgO etc.), form printed circuit, dry sintering at last, form required film.
This process efficiency height, cost are low, but microstructure is relatively poor, and the film surface of preparation is more coarse, has defective and large angle boundary in the film.The critical current density that is reached at present is too low, has only 100-1000A/cm under the 77K null field condition
2
Summary of the invention
Based on above situation, the objective of the invention is to propose a kind of method for modifying ion surface of making high-temperature superconductive device, utilize this method can reduce or eliminate the irregular status and the defective of surface to be machined, increase the evenness and the institutional framework on surface, thereby finally improve the performance of device.
Operation principle of the present invention is as follows:
Utilize ion bombardment, modification is carried out on the surface of material, surface topography, structural state and the composition of material are adjusted, can strengthen the evenness and the texture on surface, reduce the defective on surface.
1) the ion bombardment meeting influences the surface topography of material.Ion bombardment can make the pattern such as the roughness on surface change, and it is smooth to become, and also may become more coarse, this with the condition of bombardment with surperficial situation and form relevant.The top layer nonequilibrium state phonon distribution that ion bombardment causes can promote the surface migration of particle greatly, and the atom of the close surface of solids is escaped, and will produce very big influence to size, density and the texture orientation of particle in the material like this.
2) ion bombardment influences the structural state and the composition of material surface.When the ion bombardment surface of solids, ion can with the surface of solids generation sputtering phenomenon of having an effect, according to Sigmund atom cascade collision theory, sputtering raste is defined as the atomicity that the sputter from this face of each ion that incides target is got off, because the atomic mass of each constituent atoms, nuclear prevention cross section and sputter threshold energy etc. is different in the solid, the sputtering raste of each component can create a difference, promptly there is " preferential sputtering " phenomenon, like this, the structural state of material surface and component can change before and after sputter.
3) skin effect of ion bombardment also shows the defective that can reduce in the material.May there be blemish such as impurity particle, crackle, cavity in surface at material, when ion bombardment solid surperficial, the foreign particle that is adsorbed on the surface is not because firm with surface combination, be easy to obtain ion escape with the part of energy and then from the surface of solids, simultaneously, some atoms at the surface of solids may obtain bigger kinetic energy, further activate in solid, spread, and so just might change blemish such as crackle and cavity.
This method proposes a kind of method for modifying ion surface.This method comprises the selection proper technical conditions, utilizes the ion bombardment material surface, improves its surface microstructure, makes the surfacing of material, has required texture, and the density height on surface.
The present invention includes following steps:
1, a kind of high-quality material surface of cleaning is provided;
2, use the ion bombardment material surface, material is carried out surface modification.
The material of indication is employed various materials in the preparation high-temperature superconductive device among the present invention, and as semiconductor, metal or superconductor, the surface of material can be monocrystalline, amorphous or polycrystalline structure.The method of modifying ion surface generally adopts ion bombardment, can be sputter, also can be that ion injects.In order to improve the uniformity of ion beam sputtering, can select the ion source that suits and by the position between the bombardment material, as suitable angle and distance, the incident direction of ion beam with can be certain included angle by the normal of the material surface of sputter.Need to adopt suitable ion energy and scan mode, the residue of avoiding ion bombardment to produce is inserted the lowest point of film.Ion source can be used inert gas, also available reacting gas, or the mist of the two.Can select the cross section figure of the ion beam that suits,, also can be the strip that the freeman source produces as the circle that the Gunnar Nilsson source produces.
The present invention has the following advantages: technology is simple, easy operating, and the surface smoothness and the texture of material is improved a lot.
Description of drawings
Below in conjunction with accompanying drawing instantiation of the present invention is described in detail, wherein:
Fig. 1 is a kind of device schematic diagram that utilizes the plasma sputtering method film to be carried out surface modification;
Fig. 2 is a kind of device schematic diagram that utilizes ion beam sputtering film to be carried out surface modification;
Fig. 3 is a kind of schematic cross-section of high-temperature superconductor film conductor.
Embodiment
Embodiment 1
With plasma sputtering to LaAlO
3Film carries out modifying ion surface
The Ni with biaxial texture of cleaning with on deposit LaAlO with the method for adopting non-vacuum process with biaxial texture
3Buffer film is put into the reative cell with high vacuum with the sample that makes like this, carries out plasma sputtering, device schematic diagram such as Fig. 1 of its reative cell, and wherein 1 is sample, and 2 is specimen holder, and the base vacuum of reative cell is 10
-3-10
-4Pa adds at the electrode two ends and the voltage of 400-600V pours argon gas and aura then that the power of plasma is 75W when 13.65MHz, the time of aura is 1min.At film LaAlO through modification
3Last growth ybco film, and add passivation layer and protective layer thereon, schematic cross-section such as Fig. 3 of the high-temperature superconductor film conductor of acquisition, wherein 31 for having the Ni substrate of biaxial texture, and 32 is LaAlO
3Resilient coating, 33 is the superficial layer behind the ion modification, and 34 is ybco film, and 35 is passivation layer, and 36 is protective layer, this conductor has higher superconductivity.
Embodiment 2
Utilize ion beam sputtering that Y stabilizing zirconia (YSZ) film is carried out modifying ion surface
Method with adopting non-vacuum process on the Ni-Cr polycrystalline band with flexible textured substrate of cleaning deposits the resilient coating YSZ film with biaxial texture, utilize ion beam bombardment that the YSZ film is carried out modification again, device schematic diagram such as Fig. 2 of its reative cell, wherein 3 is the bombarding ion source, 1 is sample, and 2 is specimen holder.Ar with 10mA, 300V
+Ion beam bombardment, ion energy are in the magnitude of 1250ev, and the synchronous swing of system is realized the mechanical scanning of ion beam at platform.Passing through the ybco film of growing on the YSZ film of modification; and add passivation layer and protective layer thereon; schematic cross-section such as Fig. 3 of the high-temperature superconductor film conductor that obtains; wherein 31 for having the Ni-Cr substrate of biaxial texture, and 32 is the YSZ resilient coating, and 33 is the superficial layer behind the ion modification; 34 is ybco film; 35 is passivation layer, and 36 is protective layer, and this conductor has higher superconductivity.
Embodiment 3
Utilize ion beam sputtering to Al
2O
3Substrate carries out modifying ion surface
Device schematic diagram such as Fig. 2 of reative cell, wherein 3 is the bombarding ion source, 1 sample is the Al of cleaning
2O
3Substrate, 2 is specimen holder.The background air pressure of reative cell is 8.5 * 10
-4Pa is with the Ar of 60mA, 5000V
+Ion beam bombardment, ion energy are in the magnitude of 1000ev, and the synchronous swing of system is realized the mechanical scanning of ion beam at platform.Al through modification
2O
3Substrate surface is smooth, does not have tangible cut, pit or other blemish.
Embodiment 4
Utilize ion beam sputtering that the YBCO bulk is carried out modifying ion surface
Device schematic diagram such as Fig. 2 of reative cell, wherein 3 is the bombarding ion source, and 1 sample is the YBCO bulk of cleaning, and 2 is specimen holder.The background air pressure of reative cell is 6 * 10
-4Pa is with the Ar of 60mA, 5000V
+Ion beam bombardment, ion energy are in the magnitude of 1000ev, and the synchronous swing of system is realized the mechanical scanning of ion beam at platform.The result shows that ion beam sputtering has improved the evenness and the density on YBCO bulk surface, has reduced face crack.
List of references:
[1]P.C.McIntyre，Journal?of?Applied?Physics，71(4)，1868(1992)；
[2]L.D.Woolf?etc，Applied?Physics?Letter，58(5)，543(1991)；
[3] Zhang Qirui, " high-temperature superconductor is electrical ", publishing house of Zhejiang University, 1992.
Claims (3)
1. method for modifying ion surface of making the high-temperature superconductor film conductor, described method is as follows:
A kind of high-quality material surface for the preparation high-temperature superconductive device of cleaning is provided, and this material is semiconductor or metal;
Adopt the described material surface of ion bombardment that material is carried out surface modification, described bombardment is a sputtering method, or ion injection method, and material is carried out surface modification, and the surface of described material is monocrystalline, amorphous or polycrystalline structure;
Select the position between suitable ion source and the quilt bombardment material, suitable angle and distance;
Select the incident direction of ion beam and be certain included angle by the normal of the material surface of sputter;
Select the used gas of ion source, use inert gas, or use reacting gas, or the mist of the two;
Select the cross section figure of suitable ion beam, or the circle that produces for the Gunnar Nilsson source, or be the strip of freeman source generation;
It is characterized in that modification is carried out in the substrate of high-temperature superconductor film conductor or the surface on barrier layer, wherein:
Described sputter is that the using plasma sputtering method is to LaAlO
3Film carries out modifying ion surface, and described method of modifying is as follows:
Produce LaAlO
3Buffer film: the method with adopting non-vacuum process on the Ni substrate with biaxial texture of cleaning deposits the LaAlO with biaxial texture
3Buffer film;
With the LaAlO that produces
3Buffer film is put into the reative cell with high vacuum, carries out plasma sputtering, and wherein the base vacuum of reative cell is 10
-3-10
-4Pa adds at the electrode two ends and the voltage of 400-600V pours argon gas and aura then that the power of plasma is 75W when 13.65MHz, the time of aura is 1min;
At film LaAlO through modification
3Last growth ybco film, and add passivation layer and protective layer thereon, the high-temperature superconductor film conductor of acquisition.
2. method of modifying as claimed in claim 1 is characterized in that modification is carried out in the substrate of high-temperature superconductor film conductor or the surface on barrier layer, wherein,
Described sputter is to adopt ion beam sputtering that the Y stabilized zirconia film is carried out modifying ion surface, and described method of modifying is as follows:
Produce the Y stabilized zirconia film: the method with adopting non-vacuum process on the Ni-Cr substrate with flexible textured substrate of cleaning deposits the resilient coating Y stabilized zirconia film with biaxial texture;
Utilize ion beam bombardment that the Y stabilized zirconia film is carried out modification again, wherein, adopt the Ar of 10mA, 300V
+Ion beam bombardment, ion energy are in the magnitude of 1250ev, and the synchronous swing of simultaneity factor is realized the mechanical scanning of ion beam at platform;
Pass through the ybco film of growing on the Y stabilized zirconia film of modification, and adding passivation layer and protective layer thereon, the high-temperature superconductor film conductor of acquisition.
3. method of modifying as claimed in claim 1 is characterized in that modification is carried out on the surface of the used base material of preparation high temperature superconducting film, wherein,
Described sputter is to utilize ion beam sputtering to Al
2O
3Substrate carries out modifying ion surface, and the background air pressure of reative cell is 8.5 * 10
-4Pa is with the Ar of 60mA, 5000V
+Ion beam bombardment, ion energy are in the magnitude of 1000ev, and the synchronous swing of system is realized the mechanical scanning of ion beam at platform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011404329A CN100336237C (en) | 2001-12-06 | 2001-12-06 | Method for modifying ion surface for making high-temperature superconductive device |
Applications Claiming Priority (1)
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| CN100458981C (en) * | 2006-10-09 | 2009-02-04 | 西南交通大学 | Method for preparing buffer layer of conductor of high-temperature superconductor coat |
| CN106057975A (en) * | 2016-07-19 | 2016-10-26 | 苏州阿特斯阳光电力科技有限公司 | PERC solar cell manufacturing method |
| CN111799362A (en) * | 2020-07-10 | 2020-10-20 | 北京航空航天大学 | Method for surface modification of material for manufacturing high-temperature superconducting device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6456353A (en) * | 1987-08-26 | 1989-03-03 | Seiko Epson Corp | Superconductive material |
| JPH01286982A (en) * | 1988-05-11 | 1989-11-17 | Seiko Epson Corp | High-temperature superconductor and production thereof |
| JPH022742A (en) * | 1988-06-17 | 1990-01-08 | Nippon Syst Design Kk | Bi-directional serial data communication method |
| US4966885A (en) * | 1989-08-25 | 1990-10-30 | At&T Bell Laboratories | Method of producing a device comprising a metal oxide superconductor layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6456353A (en) * | 1987-08-26 | 1989-03-03 | Seiko Epson Corp | Superconductive material |
| JPH01286982A (en) * | 1988-05-11 | 1989-11-17 | Seiko Epson Corp | High-temperature superconductor and production thereof |
| JPH022742A (en) * | 1988-06-17 | 1990-01-08 | Nippon Syst Design Kk | Bi-directional serial data communication method |
| US4966885A (en) * | 1989-08-25 | 1990-10-30 | At&T Bell Laboratories | Method of producing a device comprising a metal oxide superconductor layer |
Non-Patent Citations (1)
| Title |
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| Nuclear Instruments and Methods in Physics Research B N. Bordes,S. N. Basu1,A. D. Rollett and M. Nastasi,1399.1403,Properties of thin.film YBa2Cu3O7.x superconductorsgrownon ion.irradiated SrTiO3 substrates 1991 * |
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