CN103500793A - Method for manufacturing magnesium diboride superconducting thin film micro-structure through annealing - Google Patents
Method for manufacturing magnesium diboride superconducting thin film micro-structure through annealing Download PDFInfo
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- CN103500793A CN103500793A CN201310415603.3A CN201310415603A CN103500793A CN 103500793 A CN103500793 A CN 103500793A CN 201310415603 A CN201310415603 A CN 201310415603A CN 103500793 A CN103500793 A CN 103500793A
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Abstract
The invention discloses a method for manufacturing a magnesium diboride superconducting thin film micro-structure through annealing. According to the method, electron beams are used for annealing a magnesium diboride precursor film with micro-structure patterns in a vacuum. The magnesium diboride precursor film with the micro-structure patterns is an Mg/B multi-layer film manufactured with a film masking method. Elementary substances of magnesium and boron in the precursor film undergo a chemical reaction in annealing time of a second order of magnitude, and finally, the magnesium diboride superconducting thin film micro-structure with the conversion temperature higher than 35K is generated.
Description
Technical field
The present invention relates to a kind of preparation method of superconducting thin film micro-structural, particularly the short annealing of a kind of employing electron beam prepares magnesium diboride (MgB
2) method of superconducting thin film micro-structural.
Background technology
MgB
2superconducting thin film is mainly used in the processing of two class superconductive electronic devices in person in electronics, a class is based on the Superconducting Quantum device of Josephson superconducting junction, as superconducting quantum interference device (SQUID) (SQUID), Superconducting Quantum switch etc.; Another kind of is the microwave device that utilizes superconduction low-loss character to make, as resonator, filter etc.At present, based on MgB
2the preparation of the micro-structurals such as the Josephson knot of film be mostly according to the processing sequence that first prepares preparation micro-structural after superconducting thin film, complete (referring to 1, the film preparation of MgB2 superconductor and the realization of superconductive device thereof, Wu Ke, remaining enhancing, Zhang Xiedong, Nie Ruijuan, Wang Furen, Peking University's journal (natural science edition), the 43rd volume, the 5th phase, in September, 2007; Referring to 2, Nano-bridges based on the superconducting MgB2thin films, M.Gregor, R.Mic ˇ unek, T.Plecenik, et al., Physica C468 (2008) 785 – 788; Referring to 3, All-MgB2tunnel junctions with aluminum nitride barriers, Hisashi Shimakage, Kazuya Tsujimoto, Zhen Wang, APPLIED PHYSICS LETTERS86,072512(2005)).In this preparation process owing to relating to the technique such as surface treatment, gluing, development, burn into are removed photoresist, ion etching, superconducting thin film inevitably can contact with liquid, steam, energetic ion etc., and the superconductivity variation that these contacts will make film quench even.
Chinese patent 201110112739.8 " preparing magnesium diboride superconducting thin film by electron beam annealing method " and 2011120328538.1 " electron beam annealing prepares the method for magnesium diboride Josephson junction " have proposed respectively employing electron beam annealing method and have prepared magnesium diboride superconducting thin film and magnesium diboride Josephson junction.
The method of patent 201110112739.8 is: the pioneer's film prepared is positioned in electron beam annealing equipment, adjusts beam voltage, line and beam spot diameter,, adjust annealing time, carry out short annealing, prepare MgB
2superconducting thin film.Pioneer's film that this patent is used is periodic structure, and [Mg (120
)+B (80
)]
nmultilayer film, in this structural formula, each periodic structure of the content representation pioneer's film in square brackets is 120 by thickness
mg layer and thickness be 80
the B layer form, i.e. deposition ground floor Mg (120 on substrate
), then deposit second layer B (80
), the thickness of each periodic structure is 200
the periodicity that N is periodic structure, be positive integer, and its value depends on required film thickness, and for example: if pioneer's film thickness is 20nm, the value of N is 1; If pioneer's film thickness is 10000nm, the value of N gets 500, by that analogy.Can the life cycle structure be also that [Mg (150
)+B (100
)]
nmultilayer film is pioneer's film.
The method of patent 2011120328538.1 is: the sandwich-type magnesium diboride Josephson junction pioneer film prepared is positioned in electron beam annealing equipment, adjust beam voltage, line and beam spot diameter,, adjust annealing time, carry out short annealing, prepare MgB
2-X-MgB
2the SNS type of structure or SIS type magnesium diboride Josephson junction, X represents standard conductor layer N or insulating barrier I.The sandwich-type that this patent is used (or claiming sandwich type) magnesium diboride Josephson junction pioneer membrane structure is [Mg/B]-X-[Mg/B].[Mg/B]-X-[Mg/B] preparation method of pioneer's film is: first deposit bottom [Mg/B] pioneer film on substrate, then deposit barrier layer X thereon, then on barrier layer X deposited top layer [Mg/B] pioneer film.X is standard conductor layer N or insulating barrier I, and the X layer thickness is determined according to different barrier layer materials.[Mg/B] pioneer film is [Mg (12nm)+B (8nm)] M multilayer film, in this structural formula, the B layer that the Mg layer that each periodic structure of content representation pioneer's film in square brackets is 12nm by thickness and thickness are 8nm forms, deposit ground floor Mg (12nm) on substrate, deposit second layer B (8nm), the thickness of each periodic structure is 20nm again; The periodicity that M is periodic structure, be positive integer, and its value depends on required film thickness, and for example: if pioneer's film thickness is 20nm, the value of M is 1; If pioneer's film thickness is 10000nm, the value of M gets 500, by that analogy.[Mg/B] pioneer film can be also periodic structure [Mg (15nm)+B (10nm)]
mmultilayer film.
From the inventive method of Chinese patent 201110112739.8 and 2011120328538.1, can find out, the precursor film that these two kinds of patents are used is all directly on fully exposed substrate, to deposit, whole precursor film is continuous, there is no micro-structural on precursor film, can not form the magnesium diboride superconducting thin film with micro-structural after annealing.Prepare the superconducting thin film micro-structural and also must on the superconducting thin film that uses patent 201110112739.8 and 2011120328538.1 prepare, carry out the techniques such as gluing, exposure, development, burn into remove photoresist, ion etching, superconducting thin film just inevitably can contact with liquid, steam, energetic ion etc. like this, and the superconductivity variation that finally can cause prepared film microstructure is quench even.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, propose a kind of method that adopts the electron beam short annealing to prepare magnesium diboride superconducting thin film micro-structural.The present invention only just can directly be prepared into the superconducting thin film micro-structural through a short annealing, can avoid contacting of superconducting thin film and liquid, steam, energetic ion etc.
The inventive method is as follows:
The magnesium diboride precursor film with microstructure graph prepared is positioned in the vacuum specimen chamber of electron beam annealing equipment, adopt electron beam to be annealed to the magnesium diboride precursor film with microstructure graph, magnesium make precursor film in the annealing time of number of seconds magnitude in, boron simple substance generation chemical reaction, finally generate magnesium diboride superconducting thin film micro-structural.The described Mg/B multilayer film of magnesium diboride precursor film for adopting mask method to prepare with microstructure graph.
The present invention adjusts beam voltage, line and beam spot diameter,, adjusts annealing time, carries out short annealing, can prepare magnesium diboride superconducting thin film micro-structural.
Precursor film preparation method of the present invention is: the hollowed-out mask version that will have micro-structural with spring pressuring plate or high temperature resistant adhesive tape is fixed on naked substrate, then put into the film preparing systems such as electron beam coater or magnetron sputtering coater or pulse laser coating machine, according to Mg layer and B layer thickness ratio Mg:B=3:2, be that atomic ratio is Mg:B=1:2, evaporation has periodic structure for [Mg+B]
nthe micro-structural multilayer film, the periodicity that N is periodic structure, N is positive integer.
The concrete steps of the inventive method are as follows:
1. preparation has the magnesium diboride precursor film of microstructure graph: the hollowed-out mask version that will have micro-structural with spring leaf or high temperature resistant adhesive tape is fixed on naked substrate, then put into the film preparing systems such as electron beam coater or magnetron sputtering coater or pulse laser coating machine, according to thickness proportion Mg:B=3:2, be that atomic ratio is Mg:B=1:2, prepare and there is periodic structure for [Mg+B]
nthe micro-structural multilayer film.The periodicity that N is periodic structure, N is positive integer.Film thickness is monitored by quartz crystal thin film coating controller.
Concrete steps are as follows:
(1) naked substrate is fixed on the sample workpiece platform;
(2) the hollowed-out mask version that will have a micro-structural with spring leaf or high temperature resistant adhesive tape is fixed on naked substrate;
(3) the sample workpiece platform is positioned in film preparing system;
(4) treat that in system, vacuum degree reaches 10
-5after the Pa order of magnitude, open quartz crystal thin film coating controller;
(5) according to thickness proportion Mg:B=3:2(, be that atomic ratio is Mg:B=1:2) evaporation periodic structure [Mg+B]
nmultilayer film, according to the Mg layer of each periodic structure of magnesium diboride precursor film and the thickness of B layer, at first deposit ground floor B film on naked substrate, deposition second layer Mg film on ground floor B film, then deposit again the 3rd layer of B film on second layer Mg film, the 4th layer of Mg film of deposition on the 3rd layer of B film by that analogy, stops plated film after the numeral on quartz crystal thin film coating controller display floater reaches required magnesium diboride precursor film thickness.For example: if pioneer's film periodic structure is that [Mg (120
)+B (80
)]
n, mean that each periodic structure of pioneer's film is 120 by thickness
mg layer and thickness be 80
the B layer form, i.e. deposition ground floor B (80 on substrate
), then deposit second layer Mg (120
), the thickness of each periodic structure is 200
the periodicity that N is periodic structure, be positive integer, and its value depends on required film thickness, and for example: if pioneer's film thickness is 20nm, the value of N is 1; If pioneer's film thickness is 10000nm, the value of N gets 500, by that analogy.Can the life cycle structure be also that [Mg (150
)+B (100
)]
ndeng multilayer film, it is pioneer's film;
(6) prepared by precursor film.
2. naked substrate identical with the described naked backing material of step 1, that size is identical is put on the removable work stage of electron beam process equipment sample room, described naked substrate is the substrate that there is no deposit film.Close sample room and start vacuum pump, the vacuum degree in sample room is higher than 1.0 * 10
-2during Pa, continue the operation of next step;
3. select beam voltage U: accelerating voltage U can select arbitrarily in not higher than the 40kV scope, but the Effective depth penetration R of electronics in having the magnesium diboride precursor film of microstructure graph after precondition is accelerated by this voltage must be not less than the precursor film thickness h, the value of Effective depth penetration R can be used following formula to be estimated, wherein the unit of accelerating voltage U is kV, and the unit of R is nm:
4. utilize naked substrate to carry out groping of electron beam annealing condition, select suitable bundle spot, line.Electron beam line I and electron beam spot diameter of phi: electron beam line I and beam spot diameter, Φ should combine and be adjusted, obtain large as far as possible beam spot size with as far as possible little line, the principle of selecting is: can on workpiece, observe clear described bundle spot, the size of bundle spot is advisable to cover or to cover as much as possible naked substrate fully;
5. determine annealing time: according to step 3 and the selected electron beam line I of step 4 and accelerating voltage, electronic beam current and the bundle spot of Electron Beam spot size Φ setting value electron beam process equipment, by the travelling workpiece platform of electron beam process equipment, described naked substrate is moved to position under electron beam spot, starting electron beam is annealed, exposure time t1 and t2 when recording naked substrate kermesinus and Chinese red occurring in the electron beam process equipment sample room, annealing time t is chosen as t1≤t≤t2.Described " kermesinus " is " RAL3007Black red " color in " the international standard color card table of comparisons of RAL industry "; Described " Chinese red " is " RAL2001Red orange " color in " the international standard color card table of comparisons of RAL industry ".
6. precursor film annealing: take out naked substrate from the electron beam process equipment sample room, the magnesium diboride precursor film with microstructure graph is put in the position of then placing naked substrate in sample room, with electron beam, described precursor film is annealed, and annealing time is t, after having annealed, generate MgB
2the superconducting thin film micro-structural.
If the described magnesium diboride precursor film size with microstructure graph of 7 steps 6 is greater than described Electron Beam spot size, after the described precursor film annealing covered by electron beam spot, the travelling workpiece platform, the part that described precursor film is not covered by the bundle spot moves under the bundle spot, covered and annealed by electron beam, until whole described precursor film is annealed, generate MgB
2till the superconducting thin film micro-structural.
Annealing process of the present invention can complete in the electron beam process equipments such as electron beam welding machine, electron beam annealing machine.The precursor film preparation can complete in the film preparing systems such as electron beam coater or magnetron sputtering coater or pulse laser coating machine.
The present invention compared with prior art has the following advantages:
1, the present invention does not need the techniques such as gluing, exposure, development, burn into remove photoresist, ion etching, place the hollowed-out mask version with micro-structural on naked substrate, make the deposition materials steam only have the openwork part by mask just can deposit on substrate, non-openwork part has stopped that the deposition materials steam deposits on substrate.Plated film just can be prepared the precursor film with micro-structural consistent with the hollowed-out mask version after finishing on naked substrate.Thereby avoided contacting of superconducting thin film and liquid, steam, energetic ion etc., and can be by superconducting thin film and the subsynchronous generation of superconducting thin film micro-structural one, the superconductivity variation that can not cause film microstructure is quench even.
2, annealing time is short: annealing time is the number of seconds magnitude, can effectively reduce the volatilization of magnesium (Mg), prevents the loss of Mg;
3, annealing efficiency is high: the present invention prepares magnesium diboride superconducting thin film micro-structural and can complete in the annealing time of number of seconds magnitude, rapidly and efficiently.Be conducive to the preparation of high-quality magnesium diboride superconducting thin film micro-structural, reduce preparation cost.
4, warming and cooling rate is fast: temperature rate can be up to 10
8～10
9℃/s, thus specific heating, cooling procedure formed in film.
5, electric heating conversion efficiency is up to more than 90%, far above the photo-thermal transformation efficiency of laser 10%, environmental protection, low-carbon (LC).
The accompanying drawing explanation
The M-T curve that Fig. 1 is the magnesium diboride superconducting thin film micro-structural of selecting different beam voltages, different line and different annealing times etc. to obtain, in annealing process, sample vacuum chamber is 3.0 * 10
-3pa.
The SEM image of Fig. 2 magnesium diboride superconducting thin film micro-structural.
Embodiment
Embodiment mono-
The precursor film preparation of the present embodiment completes in the ZZXS-500 electron beam coater, and electron beam annealing carries out on homemade EBW-6 type electron beam welding machine.Precursor film is that [Mg (120
)+B (80
)]
2, i.e. N=2, thickness 40nm, precursor film is of a size of 10.0mm * 3.0mm, and substrate is SiC.
1, prepare precursor film: the naked substrate of SiC that (1) will be of a size of 10.0mm * 3.0mm is fixed on the sample workpiece platform; (2) the hollowed-out mask version that will have a micro-structural with spring leaf is fixed on naked substrate; (3) the sample workpiece platform is positioned in the ZZXS-500 electron beam coater, and starts extracting vacuum; (4) treat that vacuum degree is higher than 5 * 10
-5after Pa, open quartz crystal thin film coating controller; (5) evaporation B layer on substrate, treat that the numeral on quartz crystal thin film coating controller display floater is 80
after stop plated film; (6) evaporation Mg layer on the B layer, treat the numeral 120 on quartz crystal thin film coating controller display floater
after stop plated film; (7) evaporation B layer on the Mg layer, treat the numeral 80 on quartz crystal thin film coating controller display floater
after stop plated film; (8) repeating step (6); (9) take out the sample workpiece platform after the vacuum chamber temperature is down to room temperature, so far structure is that [Mg (120
)+B (80
)]
2, thickness 40nm precursor film prepared;
2. the identical naked substrate of SiC of naked substrate size of size and step 1 is positioned on the removable work stage in the electron beam welding machine sample room, when the sample vacuum chamber degree higher than 1.0 * 10
-2during Pa, continue operation as follows;
3. according to formula
Obtain the Effective depth penetration R=47nm of electronics in precursor film after being accelerated by 1.5kV voltage, be greater than the thickness 40nm of this sample thin film, therefore select beam voltage U=1.5kV.
4. select line I and beam spot size Φ: load accelerating voltage U=1.5kV, adjust electron beam line I, adjust beam spot diameter, Φ simultaneously, when line I=4.0mA, Φ=4.0mm, electron beam spot is high-visible and can cover the width range of precursor film fully.Therefore select I=4.0mA, Φ=4.0mm;
5. determine annealing time: U=1.5kV, I=4.0mA, Φ=4.0mm are set, by the travelling workpiece platform, naked substrate is moved to the bundle spot under position annealed, when annealing time is about 0.18s and 0.42s, naked substrate presents respectively kermesinus and Chinese red.Select accordingly annealing time t=0.3s;
6. take out the naked substrate of SiC, and precursor film is placed on the removable work stage in the electron beam welding machine sample room, U=1.5kV, I=4.0mA, Φ=4.0mm are set.Because the length 10.0mm of precursor film is greater than beam spot diameter, 4.0mm, therefore the travelling workpiece platform is moved, make precursor film along its length with the speed of 13mm/s at the uniform velocity by under the bundle spot, the annealing time that guarantees the precursor film every bit of take is 0.3s.The magnesium diboride superconducting thin film micro-structural that to obtain transition temperature after annealing be 35.2K, as shown in " embodiment mono-" curve in Fig. 1.Membrane structure as shown in Figure 2.
Embodiment bis-
The precursor film preparation of the present embodiment completes in the ZZXS-500 electron beam coater, and electron beam annealing carries out on homemade EBW-6 type electron beam welding machine.Precursor film is that [Mg (120
)+B (80
)]
4, i.e. N=4, thickness 80nm, precursor film is of a size of 10.0mm * 3.0mm, and substrate is SiC.
1, prepare precursor film: the naked substrate of SiC that (1) will be of a size of 10.0mm * 3.0mm is fixed on the sample workpiece platform; (2) the hollowed-out mask version that will have a micro-structural with spring leaf is fixed on naked substrate; (3) the sample workpiece platform is positioned in the ZZXS-500 electron beam coater, and starts extracting vacuum; (4) treat that vacuum degree is higher than 5 * 10
-5after Pa, open quartz crystal thin film coating controller; (5) evaporation B layer on substrate, treat that the numeral on quartz crystal thin film coating controller display floater is 80
after stop plated film; (6) evaporation Mg layer on the B layer, treat the numeral 120 on quartz crystal thin film coating controller display floater
after stop plated film; (7) evaporation B layer on the Mg layer, treat the numeral 80 on quartz crystal thin film coating controller display floater
after stop plated film; (8) repeating step (6); (9) repeating step (7), step (8) each 2 times successively; (10) take out the sample workpiece platform after the vacuum chamber temperature is down to room temperature, so far structure is that [Mg (120
)+B (80
)]
4, thickness 80nm precursor film prepared.
2. by size, the SiC naked substrate identical with the naked substrate size of step 1 is positioned on the removable work stage in the electron beam welding machine sample room, and sample room is evacuated to vacuum degree higher than 1.0 * 10
-2pa;
3. according to formula
Obtain the Effective depth penetration R=2656nm of electronics in precursor film after being accelerated by 15kV voltage, be greater than the thickness 80nm of this sample thin film, therefore select beam voltage U=15kV.
4. select I=15.0mA, Φ=11.0mm.
5. selective annealing time t=0.13s.
6. take out the naked substrate of SiC, and precursor film is placed on the removable work stage in the electron beam welding machine sample room, the travelling workpiece platform makes precursor film under the bundle spot, and by the bundle spot, is covered fully.U=15kV, I=15.0mA, Φ=11.0mm are set, and t=0.13s is annealed.The magnesium diboride superconducting thin film micro-structural that to obtain transition temperature after annealing be 36.1K, as shown in " embodiment bis-" curve in Fig. 1.Membrane structure as shown in Figure 2.
Embodiment tri-
The precursor film preparation of the present embodiment completes in the ZZXS-500 electron beam coater, and electron beam annealing carries out on homemade EBW-6 type electron beam welding machine.Precursor film is that [Mg (120
)+B (80
)]
6, i.e. N=6, thickness 120nm, precursor film is of a size of 10.0mm * 3.0mm, and substrate is Si.
1, prepare precursor film: the naked substrate of Si that (1) will be of a size of 10.0mm * 3.0mm is fixed on the sample workpiece platform; (2) the hollowed-out mask version that will have a micro-structural with spring leaf is fixed on naked substrate; (3) the sample workpiece platform is positioned in the ZZXS-500 electron beam coater, and starts extracting vacuum; (4) treat that vacuum degree is higher than 5 * 10
-5after Pa, open quartz crystal thin film coating controller; (5) evaporation B layer on substrate, treat that the numeral on quartz crystal thin film coating controller display floater is 80
after stop plated film; (6) evaporation Mg layer on the B layer, treat the numeral 120 on quartz crystal thin film coating controller display floater
after stop plated film; (7) evaporation B layer on the Mg layer, treat the numeral 80 on quartz crystal thin film coating controller display floater
after stop plated film; (8) repeating step (6); (9) repeating step (7), (8) each 4 times successively; (10) take out the sample workpiece platform after the vacuum chamber temperature is down to room temperature, so far structure is that [Mg (120
)+B (80
)]
6, thickness 120nm precursor film prepared.
2. by size, the Si naked substrate identical with the naked substrate size of step 1 placed on the removable work stage in the electron beam welding machine sample room, and sample room is evacuated to vacuum degree higher than 1.0 * 10
-2pa;
3. with embodiment bis-, select U=15kV.
4. select I=1.5mA, Φ=7.0mm.
5. selective annealing time t=0.30s.
6. take out the naked substrate of Si and precursor film is placed on the removable work stage in the electron beam welding machine sample room, U=15kV, I=1.5mA, Φ=7.0mm are set.Because the length 10mm of precursor film is greater than beam spot diameter, 7mm, therefore the travelling workpiece platform is moved, make precursor film along its length with the speed of 23mm/s at the uniform velocity by under the bundle spot, the annealing time that guarantees the precursor film every bit of take is 0.30s.The magnesium diboride superconducting thin film micro-structural that to obtain transition temperature after annealing be 35.2K, as shown in " embodiment tri-" curve in Fig. 1.Membrane structure as shown in Figure 2.
Embodiment tetra-
The precursor film preparation of the present embodiment completes in the ZZXS-500 electron beam coater, and electron beam annealing carries out on homemade EBW-6 type electron beam welding machine.Precursor film is that [Mg (150
)+B (100
)]
24, i.e. N=24, thickness 600nm, film dimensions is 10.0mm * 10.0mm, substrate is SiC.
1, prepare precursor film: the naked substrate of SiC that (1) will be of a size of 10.0mm * 10.0mm is fixed on the sample workpiece platform; (2) the hollowed-out mask version that will have a micro-structural with spring leaf is fixed on naked substrate; (3) the sample workpiece platform is positioned in the ZZXS-500 electron beam coater, and starts extracting vacuum; (4) treat that vacuum degree is higher than 5 * 10
-5after Pa, open quartz crystal thin film coating controller; (5) evaporation B layer on substrate, treat that the numeral on quartz crystal thin film coating controller display floater is 100
after stop plated film; (6) evaporation Mg layer on the B layer, treat the numeral 150 on quartz crystal thin film coating controller display floater
after stop plated film; (7) evaporation B layer on the Mg layer, treat the numeral 100 on quartz crystal thin film coating controller display floater
after stop plated film; (8) repeating step (6); (9) repeating step (7), (8) each 22 times successively; (10) take out the sample workpiece platform after the vacuum chamber temperature is down to room temperature, so far structure is that [Mg (150
)+B (100
)]
24, thickness 600nm precursor film prepared.
2. by size, the SiC naked substrate identical with the naked substrate size of step 1 placed on the removable work stage in the electron beam welding machine sample room, and sample room is evacuated to vacuum degree higher than 1.0 * 10
-2pa;
3. according to formula
Obtain the Effective depth penetration R=14781nm of electronics in precursor film after being accelerated by 40kV voltage, be greater than the thickness 600nm of this sample thin film, therefore select beam voltage U=40kV.
4. select I=14.1mA, Φ=14.0mm.
5. selective annealing time t=0.31s.
6. take out the naked substrate of SiC and precursor film is placed on the removable work stage in the electron beam welding machine sample room, the travelling workpiece platform makes precursor film under the bundle spot, and by the bundle spot, is covered fully.U=40kV, I=14.1mA, Φ=14.0mm are set, and t=0.31s is annealed.The magnesium diboride superconducting thin film micro-structural that to obtain transition temperature after annealing be 36.1K, as shown in " embodiment tetra-" curve in Fig. 1.Membrane structure as shown in Figure 2.
Embodiment five
The precursor film preparation of the present embodiment completes in the ZZXS-500 electron beam coater, and electron beam annealing carries out on homemade EBW-6 type electron beam welding machine.Precursor film is that [Mg (150
)+B (100
)]
40, i.e. N=40, thickness 1000nm, film dimensions is 10.0mm * 10.0mm, substrate is SiC.
1, prepare precursor film: the naked substrate of SiC that (1) will be of a size of 10.0mm * 10.0mm is fixed on the sample workpiece platform; (2) the hollowed-out mask version that will have a micro-structural with spring leaf is fixed on naked substrate; (3) the sample workpiece platform is positioned in the ZZXS-500 electron beam coater, and starts extracting vacuum; (4) treat that vacuum degree is higher than 5 * 10
-5after Pa, open quartz crystal thin film coating controller; (5) evaporation B layer on substrate, treat that the numeral on quartz crystal thin film coating controller display floater is 100
after stop plated film; (6) evaporation Mg layer on the B layer, treat the numeral 150 on quartz crystal thin film coating controller display floater
after stop plated film; (7) evaporation B layer on the Mg layer, treat the numeral 100 on quartz crystal thin film coating controller display floater
after stop plated film; (8) repeating step (6); (9) repeating step (7), (8) each 38 times successively; (10) take out the sample workpiece platform after the vacuum chamber temperature is down to room temperature, so far structure is that [Mg (150
)+B (100
)]
40, thickness 1000nm precursor film prepared.
2. by size, the SiC naked substrate identical with the naked substrate size of step 1 placed on the removable work stage in the electron beam welding machine sample room, and sample room is evacuated to vacuum degree higher than 1.0 * 10
-2pa;
3. according to formula
Obtain the Effective depth penetration R=14781nm of electronics in precursor film after being accelerated by 40kV voltage, be greater than the thickness 1000nm of this sample thin film, therefore select beam voltage U=40kV.
4. select I=11.0mA, Φ=13.0mm.
5. selective annealing time t=0.40s.
6. take out the naked substrate of SiC and precursor film is placed on the removable work stage in the electron beam welding machine sample room, the travelling workpiece platform makes precursor film under the bundle spot, and by the bundle spot, is covered fully.U=40kV, I=11.0mA, Φ=13.0mm are set, and t=0.40s is annealed.The magnesium diboride superconducting thin film micro-structural that to obtain transition temperature after annealing be 35.1K, as shown in " embodiment five " curve in Fig. 1.Membrane structure as shown in Figure 2.
Claims (8)
1. the method for a preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural, it is characterized in that: described preparation method is: the vacuum sample at electron beam process equipment is indoor, adopt electron beam to be annealed to the magnesium diboride precursor film with microstructure graph, make magnesium, boron simple substance generation chemical reaction in described magnesium diboride precursor film in the annealing time of number of seconds magnitude, finally generate magnesium diboride superconducting thin film micro-structural; The described Mg/B multilayer film of magnesium diboride precursor film for adopting mask method to prepare with microstructure graph.
2. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 1, it is characterized in that: the described magnesium diboride precursor film preparation method with microstructure graph is:
The hollowed-out mask version that will have microstructure graph is fixed on naked substrate, then put into the film preparing systems such as electron beam coater or magnetron sputtering coater or pulse laser coating machine, according to Mg layer and B layer thickness ratio Mg:B=3:2, be that atomic ratio is Mg:B=1:2, evaporation has periodic structure for [Mg+B]
nthe micro-structural multilayer film, the periodicity that N is periodic structure, N is positive integer.
3. according to the method for the described preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural of claim 1 or 2, it is characterized in that: the described magnesium diboride precursor film preparation method's with microstructure graph step is as follows:
(1) described naked substrate is fixed on the sample workpiece platform;
(2) the hollowed-out mask version that will have a micro-structural with spring leaf or high temperature resistant adhesive tape is fixed on described naked substrate;
(3) the sample workpiece platform is positioned in film preparing system;
(4) treat that in film preparing system, vacuum degree reaches 10
-5after the Pa order of magnitude, open quartz crystal thin film coating controller;
(5) to naked substrate plated film;
(6) after showing the magnesium diboride precursor film thickness that reaches required, quartz crystal thin film coating controller stops plated film;
(7) the precursor film taking-up prepared is stand-by, so far prepared by precursor film.
4. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 2, it is characterized in that: described evaporation periodic structure [Mg+B]
nthe method of multilayer film is according to the Mg layer of described each periodic structure of magnesium diboride precursor film and the thickness of B layer, at first deposit ground floor B film on naked substrate, deposition second layer Mg film on ground floor B film, then deposit again the 3rd layer of B film on second layer Mg film, the 4th layer of Mg film of deposition on the 3rd layer of B film, by that analogy.
5. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 2, it is characterized in that: the described hollowed-out mask version with microstructure graph is close on naked substrate.
6. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 2, it is characterized in that: described precursor film preparation system is electron beam coater or magnetron sputtering coater or pulse laser coating machine.
7. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 1, it is characterized in that: the described method for annealing step with magnesium diboride precursor film of microstructure graph is:
(1) naked backing material that will be used with preparing precursor film naked substrate identical, that size is identical is put on the removable work stage of electron beam process equipment sample room, and described naked substrate is the substrate of deposit film not; Close sample room and start vacuum pump, the vacuum degree in sample room is higher than 1.0 * 10
-2during Pa, continue the operation of next step;
(2) select beam voltage U: accelerating voltage U selects arbitrarily in not higher than the 40kV scope, but the Effective depth penetration R of electronics in having the magnesium diboride precursor film of microstructure graph after precondition is accelerated by this voltage must be not less than the precursor film thickness h, the value of Effective depth penetration R is used following formula estimation, wherein the unit of accelerating voltage U is kV, and the unit of R is nm:
(3) utilize naked substrate to carry out groping of electron beam annealing condition, select suitable electron beam line I and electron beam spot diameter of phi: with as far as possible little electron beam line I, obtain large as far as possible beam spot size, the principle of selecting is: can on workpiece, observe and know electron beam spot, the size of bundle spot be advisable to cover or to cover as much as possible naked substrate fully;
(4) determine annealing time: the selected beam voltage U according to step (2), and the selected electron beam line I of step (3) and electron beam spot diameter of phi are set accelerating voltage, electron beam line and the electron beam spot of electron beam process equipment, by the travelling workpiece platform of electron beam process equipment, described naked substrate is moved to position under electron beam spot, start electron beam and annealed; Exposure time t1 and t2 when recording naked substrate kermesinus and Chinese red occurring in the electron beam process equipment sample room, annealing time t is chosen as t1≤t≤t2; Described " kermesinus " is " RAL3007Black red " color in " the international standard color card table of comparisons of RAL industry "; Described " Chinese red " is " RAL2001Red orange " color in " the international standard color card table of comparisons of RAL industry ";
(5) precursor film annealing: take out naked substrate from the electron beam process equipment sample room, the magnesium diboride precursor film with microstructure graph is put in the position of then placing naked substrate in sample room, with electron beam, described precursor film is annealed, annealing time is t, after having annealed, generate MgB
2the superconducting thin film micro-structural;
(6) if the described magnesium diboride precursor film size with microstructure graph of step (5) is greater than described Electron Beam spot size, after the described precursor film annealing covered by electron beam spot, the travelling workpiece platform, the part that described precursor film is not covered by the bundle spot moves under the bundle spot, covered and annealed by electron beam, until whole described precursor film is annealed, generate MgB
2till the superconducting thin film micro-structural.
8. according to the method for preparing magnesium diboride superconducting thin film by electron beam annealing micro-structural claimed in claim 1, it is characterized in that: described electron beam process equipment is electron beam welding machine or electron beam annealing machine.
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| CN103904210A (en) * | 2014-02-19 | 2014-07-02 | 中国科学院电工研究所 | Method for preparing magnesium diboride superconductive Josephson junction through secondary mask method |
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