CN114898942A - YBCO viscous superconducting coating and preparation method and application thereof - Google Patents

YBCO viscous superconducting coating and preparation method and application thereof Download PDF

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Publication number
CN114898942A
CN114898942A CN202210340992.7A CN202210340992A CN114898942A CN 114898942 A CN114898942 A CN 114898942A CN 202210340992 A CN202210340992 A CN 202210340992A CN 114898942 A CN114898942 A CN 114898942A
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China
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coating
ybco
temperature
powder
superconducting
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CN202210340992.7A
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Chinese (zh)
Inventor
祝亮
鲁向阳
谢大弢
肖丽
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Peking University
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Peking University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/02Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
    • H01B12/06Films or wires on bases or cores
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Abstract

The invention discloses a YBCO adhesive coating and a preparation method thereof. The method comprises the steps of fully mixing YBCO powder and commercial DB5015 type Ag powder conductive adhesive, coating the conductive adhesive on a substrate as a coating by using a screen printing mode and the like, and then carrying out low-temperature glue curing, medium-temperature oxygen permeation treatment, surface mechanical polishing, absolute ethyl alcohol ultrasonic cleaning and nitrogen drying to obtain the YBCO viscous superconducting coating. The superconducting coating obtained by the invention has the advantages of high critical temperature of YBCO and strong binding force of Ag powder conductive adhesive, the superconducting property is excellent, the coating is firmly bound with a substrate, high-temperature treatment is not needed in the coating preparation process, and the Ag element doping can promote the c-axis oriented growth of the YBCO coating and is beneficial to improving the superconducting property of the coating.

Description

YBCO viscous superconducting coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of radio frequency superconducting accelerating cavities, and particularly relates to a YBCO viscous superconducting coating and a preparation method thereof.
Background
Radio frequency superconducting cavities have been widely used in a range of accelerator fields, such as high energy physics, nuclear physics, free electron laser, etc., due to their low surface loss, high Q-factor, and ability to operate in high duty cycle, even Continuous Wave (CW) mode. At present, most of materials for preparing the superconducting cavity adopt Nb or Nb 3 Sn, both low temperature superconductors, require liquid helium to cool the superconducting cavity during operation. However, liquid helium is a non-renewable resource, and the reserve of liquid helium in china only occupies 0.2% of the total amount of the world, and china faces a serious helium crisis challenge. The maximum critical temperature of the YBCO high-temperature superconducting material canThe superconducting cavity prepared by the material can run in the environment of liquid nitrogen, the source of the liquid nitrogen is wide, and the running and maintenance of cooling equipment are relatively simple, so that the development of the superconducting cavity prepared by the high-temperature superconducting material is an effective means for solving the helium crisis faced at present.
For radio frequency superconducting materials, the effective action area of the radio frequency electric field is between tens of nanometers and hundreds of nanometers away from the surface, so the research on radio frequency high temperature superconducting materials is mainly focused on effectively attaching a high temperature superconducting material coating on a substrate. For the preparation of the YBCO coating, the phenomenon that the bonding between the YBCO and a substrate is not firm and the film layer falls off is often faced, and the YBCO viscous superconducting coating and the preparation method thereof are provided based on the phenomenon.
Disclosure of Invention
The invention aims to provide a YBCO viscous superconducting coating and a preparation method thereof. The preparation method provided by the invention prepares the viscous superconducting coating by mixing the YBCO powder and the commercial DB5015 type Ag powder conductive adhesive, improves the film-substrate binding force between the superconducting coating and the substrate, and does not need high-temperature treatment in the whole preparation process.
The preparation method of the YBCO viscous superconducting coating provided by the invention comprises the following steps:
1) preparing Ag powder conductive adhesive, adding YBCO powder into the Ag powder conductive adhesive, and uniformly mixing to form a precursor coating;
2) coating the precursor coating in the step 1) on a substrate to prepare a precursor coating;
3) sequentially carrying out low-temperature glue curing treatment and medium-temperature oxygen permeation treatment on the precursor coating in the step 2) to obtain a superconducting coating with a rough surface;
4) polishing the superconducting coating with the rough surface in the step 3) by using a mechanical polishing mode to obtain a superconducting coating with a smooth surface;
5) and (5) carrying out ultrasonic cleaning on the superconducting coating with the smooth surface in the step 4) by using absolute ethyl alcohol, and carrying out nitrogen drying to obtain the YBCO viscous mixed superconducting coating.
In the step 1) of the method, preferably, the Ag powder conductive adhesive can be commercial DB5015 type Ag powder conductive adhesive, and is divided into a powder A component and a liquid B component, and the proportion is 3.5-5.5 g: 1 mL. The Ag powder conductive adhesive can be DB5015 type Ag powder conductive adhesive produced by Wuhan double-bond Cum sealing material Co.
In the step 1), the mass ratio of the component a of the Ag powder conductive adhesive powder to the YBCO powder in the precursor coating is preferably 1.2-2.5:1, and specifically may be 2: 1.
in the step 2), the coating method preferably includes screen printing, spin coating, or the like.
In step 2) of the above method, the substrate preferably comprises a substrate of alumina ceramic, copper, stainless steel, or the like.
In step 2) of the above method, the precursor coating should preferably be used up within 10min to avoid curing of the coating.
In the step 2), the coating thickness is not required, and the coating is properly applied according to the actual requirement of a user.
In the step 3), the low-temperature glue curing treatment and the medium-temperature oxygen permeation treatment are carried out in a quartz tube furnace.
In the step 3), preferably, the specific method for curing the low-temperature glue is to place the precursor coating in the step 2) at room temperature for 12-24 hours, heat the precursor coating to 80-150 ℃ and maintain the precursor coating for 2-4 hours, wherein the heating rate is 30-40 ℃/h.
In step 3), the background vacuum of the low-temperature glue curing treatment is preferably lower than 10 -1 Pa, so as to reduce the pollution of impurity elements in the air to the superconducting coating in the process of curing the low-temperature glue.
In step 3), the specific method of the medium-temperature oxygen permeation treatment is preferably 10 3 -10 4 Raising the temperature from 80-150 ℃ to 400-500 ℃ at the temperature raising rate of 150 ℃/h under the oxygen atmosphere of Pa, preserving the temperature for 2-5h, and then naturally cooling to the room temperature. The medium-temperature oxygen permeation treatment aims to ensure that the oxygen content in YBCO is sufficient, and is beneficial to improving the superconducting performance of a sample.
In step 4) of the above method, the mechanical polishing may be preferably performed by sanding, so as to remove surface irregularities caused during the coating process.
In the step 5), the time for ultrasonic cleaning with absolute ethanol is preferably 20 min. The purpose of ultrasonic cleaning is to remove surface contamination caused by mechanical polishing in step four. After the ultrasonic cleaning is carried out by using the absolute ethyl alcohol in the step 5), the sample is washed by using the deionized water, and then is dried by using nitrogen gas, so that residual ethyl alcohol molecules on the surface of the sample are avoided.
The YBCO viscous superconducting coating prepared by the method also belongs to the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
the YBCO viscous superconducting coating prepared on the substrate material has the advantages of high critical temperature of YBCO and strong bonding force of Ag powder conductive adhesive, the prepared superconducting coating has excellent superconducting performance, firm film-substrate bonding, and no high-temperature treatment is needed in the whole preparation process.
Drawings
FIG. 1 is a schematic representation of the XRD pattern of an adhesive superconductive coating of YBCO on an alumina ceramic substrate in accordance with the present invention.
FIG. 2 is a graphical representation of the results of a PPMS test of a viscous superconductive coating of an alumina ceramic substrate YBCO in accordance with the present invention.
FIG. 3 is a PPMS test result of an alumina ceramic substrate YBCO adhesive coating prepared with ergo1665 glue in a comparative example of the invention.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
The YBCO powders used in the following examples can be obtained according to the following conventional preparation method: selecting Y with the purity of 99.95 percent 2 O 3 99% of BaCO 3 And CuO powder as raw material according to YBa 2 Cu 3 O 7-x Mixing according to standard proportion, and grinding the powder into the granularity of 1-2 μm; in thatAnd sintering the fully mixed powder at 900 ℃ for 20 hours in an oxygen atmosphere to obtain YBCO powder.
EXAMPLE 1 preparation of viscous superconductive coating of YBCO on alumina ceramic substrate
Raw materials
DB5015 type Ag powder conductive adhesive powder A component, liquid B component, YBCO powder and alumina ceramic substrate
Preparation method
The method comprises the following steps: and (3.6) g of the Ag powder conductive adhesive powder A component is fully mixed with 1mL of the liquid B component, the mixture is stirred uniformly, and when the Ag powder conductive adhesive becomes silver gray slurry, 1.8g of YBCO powder is put into the Ag powder conductive adhesive and is mixed uniformly to form the precursor coating.
Step two: and (3) placing the alumina ceramic substrate sample with a smooth surface on a working platform, and uniformly coating the precursor coating in the first step on the alumina ceramic substrate sample in a screen printing mode to obtain a precursor coating.
Step three: putting the precursor coating obtained in the step two into a quartz tube furnace, and then vacuumizing the quartz tube furnace to 10 DEG -1 Pa; then carrying out low-temperature glue curing treatment, wherein the specific flow is that the glue is placed at room temperature for 12 hours, then the temperature is raised from the room temperature to 80 ℃ at the heating rate of 40 ℃/h and is maintained for 2 hours, and then the temperature is raised from 80 ℃ to 150 ℃ at the heating rate of 40 ℃/h and is maintained for 2 hours; and finally, carrying out medium-temperature oxygen permeation treatment, specifically, introducing oxygen into a quartz tube furnace to ensure that the oxygen partial pressure is 1600Pa, then heating the quartz tube furnace to 450 ℃ from 150 ℃ at the heating rate of 150 ℃/h, maintaining the temperature for 2h, and then naturally cooling the quartz tube furnace to room temperature to obtain the superconducting coating with the rough surface.
Step four: and (3) mechanically polishing the superconducting coating with the rough surface in the third step, specifically, respectively polishing with 500#, 1000#, 3000#, 5000#, 7000# abrasive paper until the surface is smooth and flat to obtain the superconducting coating with a smooth surface.
Step five: and (3) carrying out absolute ethyl alcohol ultrasonic cleaning on the superconducting coating with the smooth surface in the step four for 20min, then washing the surface ethyl alcohol with clear water, and finally carrying out nitrogen drying to obtain the YBCO viscous superconducting coating.
XRD analysis is performed on the YBCO viscous superconducting coating on the alumina ceramic substrate prepared in this example, and as a result is shown in fig. 1, it is found that YBCO has a good c-axis oriented growth, and in addition, there are some peaks of Ag powder conductive adhesive, which indicates that no chemical reaction occurs between YBCO and Ag powder conductive adhesive when they are mixed together, so that the high critical temperature of YBCO and the strong binding force of Ag powder conductive adhesive can be maintained.
The result of performing the PPMS test on the YBCO viscous superconducting coating on the alumina ceramic substrate prepared in this example is shown in fig. 2, and it is found that the critical temperature of the YBCO viscous superconducting coating can reach 89.4K, and the YBCO viscous superconducting coating has a higher critical temperature.
Comparative example 1 preparation of YBCO viscous superconducting coating on alumina ceramic substrate
Raw materials
ergo1665AB glue, YBCO powder, alumina ceramic substrate
Preparation method
The method comprises the following steps: 1.6g of ergo1665AB gum was taken in an AB component ratio of 10: 1, and then putting 1.8g of YBCO powder into the Ag powder conductive adhesive, and uniformly mixing to form a precursor coating.
Step two: and (3) placing the alumina ceramic substrate sample with a smooth surface on a working platform, and uniformly coating the precursor coating in the first step on the alumina ceramic substrate sample in a screen printing mode to obtain a precursor coating.
Step three: putting the precursor coating obtained in the step two into a quartz tube furnace, and then vacuumizing the quartz tube furnace to 10 DEG -1 Pa; then, carrying out low-temperature glue curing treatment, wherein the specific flow is that the temperature is increased from room temperature to 80 ℃ at the temperature increase rate of 40 ℃/h, and the temperature is maintained for 1 h; and finally, carrying out medium-temperature oxygen permeation treatment, specifically, introducing oxygen into a quartz tube furnace to ensure that the oxygen partial pressure is 1600Pa, then heating from 80 ℃ to 450 ℃ at the heating rate of 150 ℃/h, maintaining for 2h, and then naturally cooling to room temperature to obtain the superconducting coating with the rough surface.
Step four: and (3) mechanically polishing the superconducting coating with the rough surface in the third step, specifically, respectively polishing with 500#, 1000#, 3000#, 5000#, 7000# abrasive paper until the surface is smooth and flat to obtain the superconducting coating with a smooth surface.
Step five: and (3) carrying out absolute ethyl alcohol ultrasonic cleaning on the superconducting coating with the smooth surface in the step four for 20min, then washing the surface ethyl alcohol with clear water, and finally carrying out nitrogen drying to obtain the YBCO viscous superconducting coating.
The results of the PPMS tests on the YBCO viscous superconducting coating on the alumina ceramic substrate prepared in proportion are shown in figure 3, and the YBCO viscous superconducting coating is found to have no superconductivity.
The above embodiment is only an embodiment of the present invention, and is not intended to limit the present invention in any way. The fine tuning and modification made by the workers skilled in the art according to the spirit of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (10)

1. A preparation method of a YBCO viscous superconducting coating comprises the following steps:
1) preparing Ag powder conductive adhesive, adding YBCO powder into the Ag powder conductive adhesive, and uniformly mixing to form a precursor coating;
2) coating the precursor coating in the step 1) on a substrate to prepare a precursor coating;
3) sequentially carrying out low-temperature glue curing treatment and medium-temperature oxygen permeation treatment on the precursor coating in the step 2) to obtain a superconducting coating with a rough surface;
4) polishing the superconducting coating with the rough surface in the step 3) by using a mechanical polishing mode to obtain a superconducting coating with a smooth surface;
5) and (4) ultrasonically cleaning the superconducting coating with the smooth surface in the step 4) by using absolute ethyl alcohol, and drying by using nitrogen to obtain the YBCO viscous mixed superconducting coating.
2. The method of claim 1, wherein: in the step 1), the Ag powder conductive adhesive is commercial DB5015 type Ag powder conductive adhesive and comprises a powder A component and a liquid B component, and the ratio of the powder A component to the liquid B component is 3.5-5.5 g: 1 mL.
3. The method of claim 2, wherein: in the step 1), the mass ratio of the powder A component in the Ag powder conductive adhesive to the YBCO powder in the precursor coating is 1.2-2.5: 1.
4. The production method according to any one of claims 1 to 3, characterized in that: in the step 2), the coating mode comprises screen printing and a spin coating method;
the substrate includes an alumina ceramic substrate, a copper substrate, or a stainless steel substrate.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step 3), the low-temperature glue curing treatment and the medium-temperature oxygen permeation treatment are carried out in a quartz tube furnace;
the method for curing the low-temperature glue comprises the following steps: placing the precursor coating in the step 2) at room temperature for 12-24 h, heating to 80-150 ℃, and maintaining for 2-4h, wherein the heating rate is 30-40 ℃/h.
6. The production method according to any one of claims 1 to 5, characterized in that: in the step 3), the background vacuum of the low-temperature glue curing treatment is lower than 10 -1 Pa。
7. The production method according to any one of claims 1 to 6, characterized in that: in the step 3), the medium-temperature oxygen permeation treatment method comprises the following steps: at 10 3 -10 4 Raising the temperature from 80-150 ℃ to 400-500 ℃ at the temperature raising rate of 150 ℃/h under the atmosphere of Pa, preserving the temperature for 2-5h, and then naturally cooling to the room temperature.
8. The production method according to any one of claims 1 to 7, characterized in that: in the step 4), the mechanical polishing mode is sand paper polishing.
9. The production method according to any one of claims 1 to 8, characterized in that: in the step 5), the time for carrying out ultrasonic cleaning on the absolute ethyl alcohol is 20 min.
10. A viscous superconductive YBCO coating prepared by the process of any one of claims 1 to 9.
CN202210340992.7A 2022-04-02 2022-04-02 YBCO viscous superconducting coating and preparation method and application thereof Pending CN114898942A (en)

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CN108752048A (en) * 2018-06-29 2018-11-06 西北有色金属研究院 A kind of preparation method of YBCO composite graphites ene coatings

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