CN103915215A - Co ball Nb film heterostructure superconducting material and preparation method thereof - Google Patents
Co ball Nb film heterostructure superconducting material and preparation method thereof Download PDFInfo
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- CN103915215A CN103915215A CN201410150217.0A CN201410150217A CN103915215A CN 103915215 A CN103915215 A CN 103915215A CN 201410150217 A CN201410150217 A CN 201410150217A CN 103915215 A CN103915215 A CN 103915215A
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Abstract
The invention discloses a Co ball Nb film heterostructure superconducting material which comprises a substrate, an Nb film and a Co hollow ball array film. The Nb film is located on the substrate, and covered with the Co hollow ball array film. The Co hollow ball array film is of a hexagonal honeycomb array formed by tightly arraying a plurality of Co hollow balls layer by layer. According to the Co ball Nb film heterostructure superconducting material, a magnetic Co material and an Nb superconducting film material form the heterostructure nanostructured material, the superconducting transformation temperature and critical current density can be adjusted and controlled by an applied magnetic field or electric field, and therefore the superconductivity of the Nb film is adjusted and controlled through the magnetic domain form. The invention further discloses a preparation method for the Co ball Nb film heterostructure superconducting material.
Description
Technical field
The present invention relates to a kind of nano-heterogeneous structure material, be specifically related to a kind of Co ball Nb film heterostructure superconductor.The invention still further relates to a kind of preparation method of Co ball Nb film heterostructure superconductor.
Background technology
Superconduction and magnetic are the very important two kinds of cooperative phenomenons of Condensed Matter Physics.In ferromagnet, due to the inhibitory action of ferromagnetic internal magnetic field to superconductivity, ferromagnetic and superconduction is generally considered to be inconsistent.In block materials, ferromagnetic and superconduction is difficult to coexist; But utilize artificial preparation ferromagnetic/superconductor composite system, be but easy to realize coexisting of ferromagnetic and superconduction.Superconduction, due to the quantum coherence effect of its distinctive zero resistance current-carrying and superconducting condensation, has just shown its wide application prospect to people since finding.
But existing superconductor still has many obstacles to exist on practical road, especially aspect the Effective Regulation of superconductivity.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Co ball Nb film heterostructure superconductor, and it can regulate and control its superconducting characteristic by external magnetic field or electric current.
For solving the problems of the technologies described above, the technical solution of Co ball Nb film heterostructure superconductor of the present invention is:
Comprise substrate, Nb film, Co array membrane of hollow ball, Nb film is positioned on substrate, and Co array membrane of hollow ball is covered on Nb film; Described Co array membrane of hollow ball is hexagonal honeycomb array by multiple Co hollow ball individual layer close-packed arrays.
Described substrate is HR-Si substrate; The thickness of described Nb film is 70～200nm; The diameter of described Co hollow ball is 500～2000nm, and wall thickness is 20～100 nm.
Described Co hollow ball is provided with perforate, between the hole of adjacent C o hollow ball, is interconnected.
The present invention also provides a kind of preparation method of Co ball Nb film heterostructure superconductor, and its technical solution is, comprises the following steps:
The first step, substrate is cleaned;
Described cleaning method is:
Operation one, substrate is placed in to acetone ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation two, substrate is placed in to absolute ethyl alcohol ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation three, substrate was placed in to distilled water ultrasonic cleaning after 30 minutes, is placed in absolute ethyl alcohol stand-by; The stand-by time is not more than 1 month.
Second step, synthetic Nb film;
Substrate is put into vacuum magnetron sputtering film plating machine; Nb target is positioned over to magnetron sputtering target position, vacuumizes, carry out sputter coating, synthetic Nb film;
The sputtering power of described sputter coating is 70 watts, and the pre-sputtering time is 5000～9000 seconds, and the sputtering sedimentation time is 1500～5000 seconds;
Described Nb target purity is 99.999%;
The 3rd step, on the substrate that is coated with Nb film synthetic colloidal crystal template;
Adopt liquid-vapor interface synthetic method, make colloidal spheres invest substrate surface, form colloidal crystal template;
The concrete grammar of described synthetic colloidal crystal template is:
First, colloidal spheres solution is mixed with absolute ethyl alcohol and deionized water, form mixed solution, then mixed solution is injected in syringe;
The volume ratio of described colloidal spheres solution and absolute ethyl alcohol and deionized water is:
Be the colloidal spheres of 2 microns for diameter, colloidal spheres solution: absolute ethyl alcohol is 1:1;
Be the colloidal spheres of 1 micron for diameter, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:1:2;
The colloidal spheres that is 500nm for diameter, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:3:4.
The polystyrene colloid crystalloid solution that described colloidal spheres solution is mass ratio 10%;
Then, get a substrate with Nb film, on substrate except a corner, all layer overlay deionized waters;
Subsequently, syringe is not had on substrate one end of deionized water start iterative method, in the time that the side edge of mixed solution and deionized water is touched, mixed solution is at edges of substrate and deionized water generation interface interaction, under capillary effect, colloidal spheres floats on liquid surface, the nano-structure film of formation rule;
Described colloidal spheres is that diameter is the polystyrene colloid ball of 500～2000 nanometers.
Finally, unnecessary deionized water is siphoned away, thus on substrate the colloidal crystal template of formation rule.
The 4th step, synthetic Co array membrane of hollow ball;
Step 1, magnetron sputtering C o film;
The substrate with colloidal crystal template that the 3rd step is synthetic is placed in vacuum magnetron sputtering film plating machine, and Co target is positioned over to magnetron sputtering target position; Vacuumize, carry out sputter coating;
The sputtering power of described sputter coating is 50 watts, 100 seconds pre-sputtering time, sputtering time 1000～3000 seconds;
The purity of described Co target is 99.999%;
Step 2, removal colloidal crystal template;
The sample of step 1 synthesized is immersed in carrene, makes colloidal spheres be dissolved in carrene, remove after colloidal spheres, obtain Co ball Nb film heterostructure superconductor.
The technique effect that the present invention can reach is:
The present invention constructs magnetic Co material and Nb superconducting film material into heterogeneous structural nano structural material, can regulate and control transition temperature and the critical current density of superconduction by externally-applied magnetic field or electric field, thereby realize the superconductivity that regulates and controls Nb film by magnetic domain form.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation:
Fig. 1 is the Nb film that adopts preparation method's synthesized of the present invention, the SEM picture that utilizes field emission scanning electron microscope to obtain, and wherein particle is of a size of 20 nanometer left and right;
Fig. 2 is the ESEM picture that adopts preparation method of the present invention synthetic Co hollow ball nano-structure array on Nb film, and hollow ball diameter is 1 micron;
Fig. 3 is the change curve of the electrical resistance temperature of Co ball Nb film heterostructure superconductor of the present invention;
Fig. 4 is that Co ball Nb film heterostructure superconductor of the present invention is at 7.8k, without the change curve of the electrical resistance electric current under external magnetic field;
Fig. 5 be Co ball Nb film heterostructure superconductor of the present invention at 7.8k, external magnetic field is the change curve of the electrical resistance electric current under 400Oe;
Fig. 6 be Co ball Nb film heterostructure superconductor of the present invention at 7.8k, external magnetic field is the change curve of the electrical resistance electric current under 800Oe.
Embodiment
Co ball Nb film heterostructure superconductor of the present invention, comprises HR-Si substrate, Nb(niobium) superconducting film, Co(cobalt) array membrane of hollow ball, Nb film is positioned on substrate, and Co array membrane of hollow ball is covered on Nb film; Co array membrane of hollow ball is regular six square arrays (being hexagonal honeycomb array) by multiple Co hollow ball individual layer close-packed arrays;
The thickness of Nb film is 70～200nm;
The diameter of Co hollow ball is 500～2000nm, and wall thickness is 20～100nm;
Between the hole of Co hollow ball, be interconnected.
Co ball Nb film heterostructure superconductor of the present invention has following performance:
1, its superconducting transition temperature is: the superconducting transition temperature of Nb film (not containing Co hollow ball) is 8.3K, and the superconducting transition temperature of Co ball/Nb film heterostructure is 8.0K, as shown in Figure 3.
2, Co ball Nb film heterostructure is under 7.8K, supercurrent is with the increase of external electric field, in the time that extrinsic current reaches 1700A, sample is during from superconducting state to normal state transition, resistance jumps between superconducting state and normal state, when electric current is further increased to 2600A when above, resistance changes normal state into from superconducting state gradually, as shown in Figure 4.
3,, under the effect of outside magnetic field, along with the increase of external magnetic field, the regional extent of current jump, narrows gradually; As under 400Oe external magnetic field, the minimum current that hop region occurs is 1700A, and maximum current is 2400A, as shown in Figure 5; Under 800Oe external magnetic field, hop region minimum current is 1700A, and maximum current is 2100A, as shown in Figure 6.
The preparation method of Co ball Nb film heterostructure superconductor of the present invention, comprises the following steps:
The first step, substrate is cleaned;
Operation one, substrate is placed in to acetone ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation two, substrate is placed in to absolute ethyl alcohol ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation three, substrate is placed in to distilled water ultrasonic cleaning, and within 30 minutes, to be placed on absolute ethyl alcohol stand-by; The stand-by time is not more than 1 month;
Second step, synthetic Nb film;
The substrate cleaning up is put into high vacuum magnetron sputtering coater; Nb target is positioned over to magnetron sputtering target position, vacuumizes and make vacuum degree reach 10
-8holder; Then be filled with back end gas argon gas, back end air pressure is 8 person of outstanding talent's holders, carries out sputter coating, synthetic Nb film, as shown in Figure 1;
The sputtering power of sputter coating is 70 watts, and the pre-sputtering time is 5000～9000 seconds, and the sputtering sedimentation time is 1500～5000 seconds;
Nb target purity is 99.999%;
The 3rd step, on the substrate that is coated with Nb film synthetic colloidal crystal template;
Adopt liquid-vapor interface synthetic method, make colloidal spheres invest substrate surface, form colloidal crystal template;
Concrete grammar is:
First, colloidal spheres solution is mixed with absolute ethyl alcohol and deionized water according to certain volume ratio, more mixed solution is injected in syringe;
According to the different size of colloidal spheres, select the volume ratio of colloidal spheres solution and absolute ethyl alcohol and deionized water:
Diameter is 2 microns of colloidal spheres, colloidal spheres solution: absolute ethyl alcohol is 1:1;
Diameter is 1 micron of colloidal spheres, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:1:2;
Diameter is 500nm colloidal spheres, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:3:4;
Then, get a clean substrate with Nb film, on substrate except a corner, all layer overlay deionized waters;
Subsequently, syringe is not had on substrate one end of water start slow propelling, in the time that the side edge of mixed solution and deionized water is touched, mixed solution is at edges of substrate and deionized water generation interface interaction, under capillary effect, make colloidal spheres float on liquid surface, the nano-structure film of formation rule;
Finally, unnecessary deionized water is siphoned away with filter paper, will be on substrate the colloidal crystal template of formation rule.
Colloidal spheres solution can be the polystyrene colloid crystalloid solution of mass ratio 10%;
Colloidal spheres is that diameter is the polystyrene colloid ball of 500～2000 nanometers.
The 4th step, synthetic Co array membrane of hollow ball;
Step 1, magnetron sputtering C o film;
The substrate with colloidal crystal template that the 3rd step is synthetic is placed in high vacuum magnetron sputtering coater, and Co target is positioned over to magnetron sputtering target position; Vacuumize and make vacuum degree reach 10
-8holder; Then be filled with back end gas argon gas, back end air pressure is 8 person of outstanding talent's holders, carries out sputter coating, as shown in Figure 2;
The sputtering power of sputter coating is 50 watts, 100 seconds pre-sputtering time, sputtering time 1000～3000 seconds;
The purity of Co target is 99.999%;
Step 2, removal colloidal crystal template;
The sample of step 1 synthesized is immersed in carrene, at room temperature condition, makes colloidal spheres be dissolved in carrene at least 1 minute, remove after colloidal spheres, obtain Co ball Nb film heterostructure superconductor.
Obviously, those skilled in the art can carry out various changes and modification and not depart from the spirit and scope of the present invention preparation method of the present invention.Like this, if within these modifications of the present invention and distortion belong to the scope of the claims in the present invention and equivalent technologies thereof, the present invention is also intended to comprise these changes and distortion interior.
Claims (10)
1. a Co ball Nb film heterostructure superconductor, is characterized in that: comprise substrate, Nb film, Co array membrane of hollow ball, Nb film is positioned on substrate, Co array membrane of hollow ball is covered on Nb film; Described Co array membrane of hollow ball is hexagonal honeycomb array by multiple Co hollow ball individual layer close-packed arrays.
2. Co ball Nb film heterostructure superconductor according to claim 1, is characterized in that: described substrate is HR-Si substrate; The thickness of described Nb film is 70～200nm; The diameter of described Co hollow ball is 500～2000nm, and wall thickness is 20～100 nm.
3. Co ball Nb film heterostructure superconductor according to claim 1 and 2, is characterized in that: described Co hollow ball is provided with perforate, between the hole of adjacent C o hollow ball, is interconnected.
4. a preparation method for Co ball Nb film heterostructure superconductor claimed in claim 1, is characterized in that, comprises the following steps:
The first step, substrate is cleaned;
Second step, synthetic Nb film;
Substrate is put into vacuum magnetron sputtering film plating machine; Nb target is positioned over to magnetron sputtering target position, vacuumizes, carry out sputter coating, synthetic Nb film;
The 3rd step, on the substrate that is coated with Nb film synthetic colloidal crystal template;
Adopt liquid-vapor interface synthetic method, make colloidal spheres invest substrate surface, form colloidal crystal template;
The 4th step, synthetic Co array membrane of hollow ball;
Step 1, magnetron sputtering C o film;
The substrate with colloidal crystal template that the 3rd step is synthetic is placed in vacuum magnetron sputtering film plating machine, and Co target is positioned over to magnetron sputtering target position; Vacuumize, carry out sputter coating;
Step 2, removal colloidal crystal template;
The sample of step 1 synthesized is immersed in carrene, makes colloidal spheres be dissolved in carrene, remove after colloidal spheres, obtain Co ball Nb film heterostructure superconductor.
5. the preparation method of Co ball Nb film heterostructure superconductor according to claim 4, is characterized in that, the cleaning method of the described first step is:
Operation one, substrate is placed in to acetone ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation two, substrate is placed in to absolute ethyl alcohol ultrasonic cleaning 40 minutes, then with washed with de-ionized water repeatedly;
Operation three, substrate was placed in to distilled water ultrasonic cleaning after 30 minutes, is placed in absolute ethyl alcohol stand-by; The stand-by time is not more than 1 month.
6. the preparation method of Co ball Nb film heterostructure superconductor according to claim 4, is characterized in that, in described second step, the sputtering power of sputter coating is 70 watts, and the pre-sputtering time is 5000～9000 seconds, and the sputtering sedimentation time is 1500～5000 seconds; In described the 4th step, the sputtering power of sputter coating is 50 watts, 100 seconds pre-sputtering time, sputtering time 1000～3000 seconds.
7. the preparation method of Co ball Nb film heterostructure superconductor according to claim 4, is characterized in that, described Nb target purity is 99.999%; The purity of described Co target is 99.999%.
8. the preparation method of Co ball Nb film heterostructure superconductor according to claim 4, is characterized in that, the concrete grammar of the synthetic colloidal crystal template of described the 3rd step is:
First, colloidal spheres solution is mixed with absolute ethyl alcohol and deionized water, form mixed solution, then mixed solution is injected in syringe;
Then, get a substrate with Nb film, on substrate except a corner, all layer overlay deionized waters;
Subsequently, syringe is not had on substrate one end of deionized water start iterative method, in the time that the side edge of mixed solution and deionized water is touched, mixed solution is at edges of substrate and deionized water generation interface interaction, under capillary effect, colloidal spheres floats on liquid surface, the nano-structure film of formation rule;
Finally, unnecessary deionized water is siphoned away, thus on substrate the colloidal crystal template of formation rule.
9. the preparation method of Co ball Nb film heterostructure superconductor according to claim 8, is characterized in that, the volume ratio of described colloidal spheres solution and absolute ethyl alcohol and deionized water is:
Be the colloidal spheres of 2 microns for diameter, colloidal spheres solution: absolute ethyl alcohol is 1:1;
Be the colloidal spheres of 1 micron for diameter, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:1:2;
The colloidal spheres that is 500nm for diameter, colloidal spheres solution: deionized water: absolute ethyl alcohol is 1:3:4.
10. the preparation method of Co ball Nb film heterostructure superconductor according to claim 8, is characterized in that the polystyrene colloid crystalloid solution that described colloidal spheres solution is mass ratio 10%; Described colloidal spheres is that diameter is the polystyrene colloid ball of 500～2000 nanometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105990512A (en) * | 2016-06-24 | 2016-10-05 | 李志刚 | Polystyrene colloidal sphere and niobium film composite heterogeneous structure superconducting material and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050019616A1 (en) * | 2003-07-21 | 2005-01-27 | Foltyn Stephen R. | Buffer layer for thin film structures |
| CN102870244A (en) * | 2010-03-31 | 2013-01-09 | 美国超导体公司 | Thick oxide film by single coating |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050019616A1 (en) * | 2003-07-21 | 2005-01-27 | Foltyn Stephen R. | Buffer layer for thin film structures |
| CN102870244A (en) * | 2010-03-31 | 2013-01-09 | 美国超导体公司 | Thick oxide film by single coating |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105990512A (en) * | 2016-06-24 | 2016-10-05 | 李志刚 | Polystyrene colloidal sphere and niobium film composite heterogeneous structure superconducting material and preparation method |
| CN105990512B (en) * | 2016-06-24 | 2018-07-03 | 李志刚 | Polystyrene colloid ball and niobium film composite heterogenous junction structure superconductor and preparation method |
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