CN112830783A - Method for improving performance of composite block by doping YBCO with graphene oxide - Google Patents
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Abstract
The invention discloses a method for improving the performance of a composite block by YBCO doped graphene oxide, which comprises the following steps: preparing precursor powder; pressing the mixed precursor block; and (5) sintering. The invention has the beneficial effects that: the composite block prepared by the method reduces the porosity of the single domain YBCO block, and oxygen functional groups released by oxidized graphene enter the YBCO during high-temperature reaction, so that the carrier concentration of the block is increased, and the block has higher critical transition temperature and higher critical current density; the composite block material obtained by adopting the doping preparation method has better toughness, and greatly makes up the disadvantage of the YBCO block material in the aspect of mechanical strength; the method has the advantages of simplicity, easy realization, convenient control and the like, and provides possibility for mass industrial production of the composite block.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of high-temperature superconducting materials, in particular to a method for improving the performance of a composite block by YBCO doped graphene oxide.
[ background of the invention ]
Yttrium Barium Copper Oxide (YBCO) is used as a second-generation high-temperature superconductor, and has the advantages of high critical magnetic field, high critical current density and the like when the superconducting critical transition temperature reaches 92K. The preparation technology of the bulk material is always a research hotspot in the field of superconducting materials. At present, a Sol-Gel method is adopted to prepare YBCO precursor powder, and a dopant of the YBCO precursor powder can also be mixed into precursor liquid to obtain the YBCO precursor liquid containing the dopant. Forming a stable transparent sol system in the solution, aging the sol, and slowly polymerizing the colloidal particles to form gel. And drying, sintering and curing the gel to prepare a sample with the required YBCO dopant. But has strong requirements on the state and content of the dopant, and the preparation method of the doped compound is too complicated and is not suitable for mass industrial production. The YBCO superconducting block can form micro cracks during processing, and the cracks are easy to extend and amplify when the YBCO superconducting block is applied in a strong magnetic field environment. On the other hand, the mechanical strength of the material is poor; easily broken. The YBCO superconducting block material is prepared by a metal oxide whisker reinforced method. The mechanical strength is obviously improved, but the length-diameter ratio of the crystal whisker needs to be strictly controlled, and the superconducting performance of the YBCO superconducting block material is not beneficial.
Therefore, a new method for improving the performance of the YBCO doped Graphene Oxide (Graphene Oxide) composite block material is needed to solve the superconducting performance of the YBCO superconducting block material and overcome the problem that the YBCO superconducting block material has poor mechanical strength and cannot meet the requirement of large investment in engineering application.
[ summary of the invention ]
The invention discloses a method for improving the performance of a composite block by YBCO doped graphene oxide, which can solve the technical problems involved in the background technology.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for improving the performance of a composite block by YBCO doped graphene oxide comprises the following steps:
step one, preparing precursor powder;
mixing graphene oxide powder and yttrium barium copper oxide powder according to a mass ratio of 1: 100-200, mixing in proportion to obtain mixed powder;
placing the mixed powder into a ball mill for fine ball milling, and then placing the mixed powder subjected to fine ball milling into a ceramic mortar for grinding so as to uniformly mix the graphene oxide powder and the yttrium barium copper oxide powder to obtain mixed precursor powder;
step two, pressing a mixed precursor block;
taking out a certain amount of mixed precursor powder, putting the mixed precursor powder into a stainless steel die, tabletting by using a hydraulic press, applying pressure to 5Mpa for the first time, then gradually increasing the pressure to 30-45Mp according to the gradient of 5 Mpa/time, keeping the pressure applied to the stainless steel die at 30-45Mpa, and staying for 0.1h to obtain a mixed precursor block;
step three, sintering;
cleaning the surface of the mixed precursor block, then placing the mixed precursor block in a high-temperature tube furnace for crystallization heat treatment, wherein the heat treatment temperature is increased to 1000 ℃ from the normal temperature at the speed of 200 ℃/h, then introducing oxygen into the high-temperature tube furnace at the temperature of 1000 ℃ to ensure that the mixed precursor block is sintered for 6h in a circulating oxygen environment, then reducing the temperature to 990 ℃ from 1000 ℃ at the speed of 2 ℃/h, then reducing the temperature to 985 ℃ from 990 ℃ at the speed of 1 ℃/h, and finally naturally cooling to the room temperature from 985 ℃.
As a preferable improvement of the present invention, in the step one, the number of ball milling is refined to 3 times.
As a preferable improvement of the invention, in the step one, the rotating speed of the ball mill is 200r/min, and the ball milling time is 5 h.
As a preferred development of the invention, in step one, the grinding time is 2 h.
As a preferable improvement of the present invention, in the second step, the stainless steel mold is a cylindrical stainless steel mold with a diameter of 12 mm.
In a preferred improvement of the invention, in step three, the surface of the mixed precursor block is cleaned by using alcohol.
As a preferable improvement of the present invention, in the first step, the graphene oxide powder and the yttrium barium copper oxide powder are mixed according to a mass ratio of 1: 100, proportioning and mixing.
As a preferable improvement of the present invention, in the first step, the graphene oxide powder and the yttrium barium copper oxide powder are mixed according to a mass ratio of 1: 200 are mixed according to the mixture ratio.
As a preferable improvement of the present invention, in the second step, the pressure is maintained after the pressure is gradually increased to 30Mp by 5 MPa/time, and the pressure applied to the stainless steel mold is maintained at 30MPa and kept for 0.1 h.
As a preferable improvement of the present invention, in the second step, the pressure is maintained after the pressure is gradually increased to 45Mp by a gradient of 5 MPa/time, and the pressure applied to the stainless steel mold is maintained at 45MPa and kept for 0.1 h.
The method for improving the performance of the composite block by YBCO doped graphene oxide has the beneficial effects that:
1. the composite block prepared by the method reduces the porosity of the single domain YBCO block, and oxygen functional groups released by oxidized graphene enter the YBCO during high-temperature reaction, so that the carrier concentration of the block is increased, and the block has higher critical transition temperature and higher critical current density;
2. the composite block material obtained by adopting the doping preparation method has better toughness, and greatly makes up the disadvantage of the YBCO block material in the aspect of mechanical strength;
3. the method has the advantages of simplicity, easy realization, convenient control and the like, and provides possibility for mass industrial production of the composite block.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a process flow diagram of a method for improving the performance of a composite block by YBCO doped graphene oxide according to the present invention;
fig. 2 is a temperature control diagram of a third step of the method for improving the performance of the composite block by YBCO-doped graphene oxide according to the present invention.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a method for improving the performance of a composite block by YBCO-doped graphene oxide, including the following steps:
step one, preparing precursor powder;
mixing Graphene Oxide (Graphene Oxide) powder and Yttrium Barium Copper Oxide (YBCO) powder according to the mass ratio of 1: 100-200, mixing in proportion to obtain mixed powder;
placing the mixed powder into a ball mill for thinning ball milling for 3 times, wherein the rotating speed of the ball mill is 200r/min, the ball milling time is 5 hours, and then placing the mixed powder subjected to thinning ball milling into a ceramic mortar for grinding for 2 hours so as to uniformly mix the graphene oxide powder and the yttrium barium copper oxide powder to obtain mixed precursor powder;
step two, pressing a mixed precursor block;
taking out a certain amount of mixed precursor powder, putting the mixed precursor powder into a cylindrical stainless steel die with the diameter of 12mm, tabletting by using a hydraulic press, applying pressure to 5Mpa for the first time, then gradually increasing the pressure to 30-45Mp according to the gradient of 5 Mpa/time, keeping the pressure applied to the stainless steel die at 30-45Mpa, and staying for 0.1h to obtain a mixed precursor block;
step three, sintering;
and then, as shown in figure 2, cleaning the surface of the mixed precursor block by using alcohol, then placing the mixed precursor block in a high-temperature tube furnace for crystallization heat treatment, wherein the heat treatment temperature is increased from the normal temperature to 1000 ℃ at the speed of 200 ℃/h, then introducing oxygen into the high-temperature tube furnace at the temperature of 1000 ℃ to ensure that the mixed precursor block is sintered for 6h in a circulating oxygen environment, then reduced from 1000 ℃ to 990 ℃ at the speed of 2 ℃/h, reduced from 990 ℃ to 985 ℃ at the speed of 1 ℃/h, and finally naturally cooled to the room temperature from 985 ℃.
It should be further explained that the surface of the precursor block is cleaned by alcohol, so as to prevent the surface impurities from affecting the generation of the YBCO mixed block material on one hand, and prevent the surface of the sample from being oxidized on the other hand.
The present invention is described in detail below with reference to specific examples 1 and 2.
Example 1
The invention provides a method for improving the performance of a composite block by YBCO doped graphene oxide, which comprises the following steps:
step one, preparing precursor powder;
mixing 10g of graphene oxide powder and 1kg of yttrium barium copper oxide powder in a ratio to obtain mixed powder;
placing the mixed powder into a ball mill for thinning ball milling for 3 times, wherein the rotating speed of the ball mill is 200r/min, the ball milling time is 5 hours, and then placing the mixed powder subjected to thinning ball milling into a ceramic mortar for grinding for 2 hours so as to uniformly mix the graphene oxide powder and the yttrium barium copper oxide powder to obtain mixed precursor powder;
step two, pressing a mixed precursor block;
taking out 3g of precursor powder, putting the precursor powder into a cylindrical stainless steel die with the diameter of 12mm, tabletting by using a hydraulic machine, applying pressure to 5Mpa for the first time, then gradually increasing the pressure to 30Mp according to the gradient of 5 Mpa/time, keeping the pressure applied to the stainless steel die at 30Mpa and staying for 0.1h to obtain a mixed precursor block;
step three, sintering;
and then, as shown in figure 2, cleaning the surface of the mixed precursor block by using alcohol, then placing the mixed precursor block in a high-temperature tube furnace for crystallization heat treatment, wherein the heat treatment temperature is increased from the normal temperature to 1000 ℃ at the speed of 200 ℃/h, then introducing oxygen into the high-temperature tube furnace at the temperature of 1000 ℃ to ensure that the mixed precursor block is sintered for 6h in a circulating oxygen environment, then reduced from 1000 ℃ to 990 ℃ at the speed of 2 ℃/h, reduced from 990 ℃ to 985 ℃ at the speed of 1 ℃/h, and finally naturally cooled to the room temperature from 985 ℃.
Example 2
The invention provides a method for improving the performance of a composite block by YBCO doped graphene oxide, which comprises the following steps:
step one, preparing precursor powder;
5g of graphene oxide powder and 1kg of yttrium barium copper oxide powder are mixed in proportion to obtain mixed powder;
placing the mixed powder into a ball mill for thinning ball milling for 3 times, wherein the rotating speed of the ball mill is 200r/min, the ball milling time is 5 hours, and then placing the mixed powder subjected to thinning ball milling into a ceramic mortar for grinding for 2 hours so as to uniformly mix the graphene oxide powder and the yttrium barium copper oxide powder to obtain mixed precursor powder;
step two, pressing a mixed precursor block;
taking out 3g of precursor powder, putting the precursor powder into a cylindrical stainless steel die with the diameter of 12mm, tabletting by using a hydraulic machine, applying pressure to 5Mpa for the first time, then gradually increasing the pressure to 45Mp according to the gradient of 5 Mpa/time, keeping the pressure applied to the stainless steel die at 45Mpa and staying for 0.1h to obtain a mixed precursor block;
step three, sintering;
and then, as shown in figure 2, cleaning the surface of the mixed precursor block by using alcohol, then placing the mixed precursor block in a high-temperature tube furnace for crystallization heat treatment, wherein the heat treatment temperature is increased from the normal temperature to 1000 ℃ at the speed of 200 ℃/h, then introducing oxygen into the high-temperature tube furnace at the temperature of 1000 ℃ to ensure that the mixed precursor block is sintered for 6h in a circulating oxygen environment, then reduced from 1000 ℃ to 990 ℃ at the speed of 2 ℃/h, reduced from 990 ℃ to 985 ℃ at the speed of 1 ℃/h, and finally naturally cooled to the room temperature from 985 ℃.
The method for improving the performance of the composite block by YBCO doped graphene oxide has the beneficial effects that:
4. the composite block prepared by the method reduces the porosity of the single domain YBCO block, and oxygen functional groups released by oxidized graphene enter the YBCO during high-temperature reaction, so that the carrier concentration of the block is increased, and the block has higher critical transition temperature and higher critical current density;
5. the composite block material obtained by adopting the doping preparation method has better toughness, and greatly makes up the disadvantage of the YBCO block material in the aspect of mechanical strength;
the method has the advantages of simplicity, easy realization, convenient control and the like, and provides possibility for mass industrial production of the composite block.
While embodiments of the invention have been disclosed above, it is not limited to the applications set forth in the specification and the embodiments, which are fully applicable to various fields of endeavor for which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. A method for improving the performance of a composite block by YBCO doped graphene oxide is characterized by comprising the following steps:
step one, preparing precursor powder;
mixing graphene oxide powder and yttrium barium copper oxide powder according to a mass ratio of 1: 100-200, mixing in proportion to obtain mixed powder;
placing the mixed powder into a ball mill for fine ball milling, and then placing the mixed powder subjected to fine ball milling into a ceramic mortar for grinding so as to uniformly mix the graphene oxide powder and the yttrium barium copper oxide powder to obtain mixed precursor powder;
step two, pressing a mixed precursor block;
taking out a certain amount of mixed precursor powder, putting the mixed precursor powder into a stainless steel die, tabletting by using a hydraulic press, applying pressure to 5Mpa for the first time, then gradually increasing the pressure to 30-45Mp according to the gradient of 5 Mpa/time, keeping the pressure applied to the stainless steel die at 30-45Mpa, and staying for 0.1h to obtain a mixed precursor block;
step three, sintering;
cleaning the surface of the mixed precursor block, then placing the mixed precursor block in a high-temperature tube furnace for crystallization heat treatment, wherein the heat treatment temperature is increased to 1000 ℃ from the normal temperature at the speed of 200 ℃/h, then introducing oxygen into the high-temperature tube furnace at the temperature of 1000 ℃ to ensure that the mixed precursor block is sintered for 6h in a circulating oxygen environment, then reducing the temperature to 990 ℃ from 1000 ℃ at the speed of 2 ℃/h, then reducing the temperature to 985 ℃ from 990 ℃ at the speed of 1 ℃/h, and finally naturally cooling to the room temperature from 985 ℃.
2. The method for improving the performance of the composite block by the YBCO doped graphene oxide according to claim 1, wherein in the first step, the number of the ball milling for refining is 3.
3. The method for improving the performance of the composite block by the YBCO doped graphene oxide according to claim 1 or 2, wherein in the step one, the rotating speed of a ball mill is 200r/min, and the ball milling time is 5 h.
4. The method for improving the performance of the composite block by the YBCO-doped graphene oxide according to claim 1, wherein in the first step, the grinding time is 2 h.
5. The method for improving the performance of the composite block by the YBCO doped graphene oxide according to claim 1, wherein in the second step, the stainless steel mold is a cylindrical stainless steel mold with a diameter of phi 12 mm.
6. The method for improving the performance of the composite block by the YBCO doped graphene oxide as claimed in claim 1, wherein in the third step, the surface of the mixed precursor block is cleaned by alcohol.
7. The method for improving the performance of the composite block by the YBCO-doped graphene oxide according to claim 1, wherein in the first step, the graphene oxide powder and the yttrium barium copper oxide powder are mixed according to a mass ratio of 1: 100, proportioning and mixing.
8. The method for improving the performance of the composite block by the YBCO-doped graphene oxide according to claim 1, wherein in the first step, the graphene oxide powder and the yttrium barium copper oxide powder are mixed according to a mass ratio of 1: 200 are mixed according to the mixture ratio.
9. The method for improving the performance of the composite block by the YBCO doped graphene oxide according to claim 1, wherein in the second step, the pressure is kept after the pressure is gradually increased to 30Mp by 5 Mpa/time gradient, and the pressure applied to the stainless steel mold is kept at 30Mpa for 0.1 h.
10. The method for improving the performance of the composite block material by the YBCO doped graphene oxide according to claim 1, wherein in the second step, the pressure is kept after the pressure is gradually increased to 45Mp by 5 Mpa/time, and the pressure applied to the stainless steel mold is kept at 45Mpa for 0.1 h.
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Citations (3)
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| CN101745750A (en) * | 2008-12-17 | 2010-06-23 | 北京有色金属研究总院 | Brazing material used for preparing YBCO superconducting blocks with brazing method and a brazing technique thereof |
| 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 |
| US20200095167A1 (en) * | 2018-09-24 | 2020-03-26 | Imam Abdulrahman Bin Faisal University | Method of producing polycrystalline y-358 superconductor |
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2021
- 2021-01-21 CN CN202110078766.1A patent/CN112830783A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN101745750A (en) * | 2008-12-17 | 2010-06-23 | 北京有色金属研究总院 | Brazing material used for preparing YBCO superconducting blocks with brazing method and a brazing technique thereof |
| 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 |
| US20200095167A1 (en) * | 2018-09-24 | 2020-03-26 | Imam Abdulrahman Bin Faisal University | Method of producing polycrystalline y-358 superconductor |
Non-Patent Citations (1)
| Title |
|---|
| M Z GAFFOOR ET AL.: "Comparison of the Effect of Graphene and Graphene Oxide Doping on YBCO", 《JOURNAL OF PHYSICS: CONFERENCE SERIES》 * |
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