CN112811893A - Method for uniformly doping nanoparticles in high-temperature superconducting material - Google Patents
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Abstract
The invention relates to a method for uniformly doping nano particles in a high-temperature superconducting material, which comprises the following steps: (1) putting ethylene glycol into a glass container, preheating in a constant-temperature water bath or oil bath at 70-100 ℃, then pouring citric acid into the ethylene glycol in the water bath or oil bath, stirring to achieve complete mutual solubility, and then pouring nanoparticles into the mixture of the ethylene glycol and the citric acid in the water bath or oil bath, and continuously stirring to achieve uniform mixing; (2) pouring the mixture into a curing mold; (3) taking out the mixture after the mixture is completely solidified, crushing the mixture by a crusher, uniformly mixing the crushed powder with a certain proportion of single-phase high-temperature superconductor powder, and pressing the mixture into blocks; (4) putting the block into a heat treatment furnace, preserving heat for several hours, and cooling to room temperature; (5) and taking out the block, putting the block back to a heat treatment furnace, and carrying out heat treatment at the sintering temperature of the high-temperature superconductor for a certain time to achieve the purpose that the high-temperature superconductor is uniformly mixed with the nano particles, wherein the high-temperature superconductor is still a single-phase high-temperature superconductor. The invention has simple and convenient operation, high efficiency and good controllability.
Description
Technical Field
The invention belongs to the technical field of superconducting materials, and particularly relates to a method for uniformly doping nanoparticles in a high-temperature superconducting material.
Background
Superconducting materials can be divided into two categories according to the temperature range in which the superconducting phenomenon occurs: a low temperature superconductor in the liquid helium temperature region and a high temperature superconductor in the liquid nitrogen temperature region. Cryogenic superconductors have significant limitations in practical applications due to their low superconducting transition temperature and the need for extremely expensive liquid helium to operate. High temperature superconducting materials are mainly copper oxide ceramic materials, due to their large anisotropy and low carrier density, their critical current density JcLower and falls off very quickly with increasing magnetic field. Since they are ceramic materials, it is difficult to form high-quality wires or strips, thereby preventing their wide use.
Practical applications of high temperature superconductors must address one of the key issues: the critical current density and the irreversible critical magnetic strength are improved. When the flux pinning force is weak, the critical current density at high field is low, which affects the practical application of high temperature superconductors at high temperature (e.g. 77K) and high magnetic field (e.g. > 4T). One of the ways to increase is to increase the density of flux pinning centers. The nano particles which are dispersed and distributed are introduced into the high-temperature superconducting material to enable the nano particles to become effective magnetic flux pinning centers, so that the critical current density and the irreversible critical magnetic strength of the high-temperature superconducting material are effectively improved.
Hannachi et al[1]At YBa2Cu3OyIncorporation of TiO into high temperature superconductors2Nanoparticles to increase their critical current density; M.K.Ben Salem et al[2]By doping with SiO2Nanoparticles to increase YBa2Cu3OyCritical current density of the high temperature superconductor; m. hafiz et al[3]In (Bi, Pb)2Sr2Ca2Cu3O10Incorporation of CoFe into high temperature superconductors2O4Magnetic nanoparticles to increase its critical current density; n.a.a.yahya et al[4]By doping with Bi2O3Nanoparticles to increase Bi1.6Pb0.4Sr2Ca2Cu3O10Critical current density of high temperature superconductors. These studiesThere is no consideration that the nanoparticles agglomerate and the size of the nanoparticles is much smaller than that of the superconducting powder, resulting in non-uniform mixing of the two. Including one using BaCeO in the patent CN101450859B3The method for improving the performance of the Y-Ba-Cu-O high-temperature superconductor by doping the nano particles is only to mix BaCeO3Direct addition of nanoparticles to Y1.8Ba2.4Cu3.4OyThe ball milling mixing is carried out in the powder, and the problems that the agglomeration of nano particles and the extremely small size can cause uneven doping are not considered.
Agglomeration is a phenomenon in which when the force between particles of a material is much greater than gravity, the particles no longer act as constrained by gravity, but come close to each other under the influence of the force between the particles, thereby causing aggregation. When the nano particles are mixed with the high-temperature superconducting precursor powder, agglomeration occurs, and the nano particles and the high-temperature superconducting precursor powder cannot be uniformly mixed due to the fact that the nano particles and the high-temperature superconducting precursor powder are far different in size, so that the critical current density of the high-temperature superconducting composite material can be influenced. In order to obtain a high temperature superconducting composite with a high critical current density, agglomeration of nanoparticles and ununiformity of mixing must be avoided.
Disclosure of Invention
The invention aims to solve the problem of agglomeration and uneven dispersion of nanoparticles in a high-temperature superconducting material by utilizing a mixture organogel of Citric Acid (CA) and Ethylene Glycol (EG) aiming at the problem of non-uniformity of doped nanoparticles in the high-temperature superconducting material.
To achieve the above object, the present invention provides a method for uniformly doping nanoparticles in a high temperature superconducting material, comprising the steps of:
(1) weighing citric acid and ethylene glycol according to a certain proportion, putting the ethylene glycol into a glass container, preheating in a constant-temperature water bath or oil bath at 70-100 ℃, then pouring the citric acid into the ethylene glycol in the water bath or oil bath, stirring for a certain time to achieve complete mutual solubility, and then pouring a proper amount of nano-particles into the mixture of the ethylene glycol and the citric acid in the water bath or oil bath, and continuously stirring for a certain time to achieve uniform mixing;
(2) pouring the uniformly mixed mixture of the glycol, the citric acid and the nano particles into a curing mold, and then placing the curing mold into a forced air drying box for curing at the temperature of 130-150 ℃, wherein the curing time is more than 8 h;
(3) taking out the mixture after the mixture is completely solidified, crushing the mixture by using a crusher, uniformly mixing the crushed powder with a certain proportion of single-phase high-temperature superconductor powder, and pressing the mixture into blocks by using a tablet press;
(4) putting the pressed block into a heat treatment furnace, preserving the heat for a plurality of hours at the temperature of 430-500 ℃, and then cooling to room temperature;
(5) and taking out the block after heat treatment, compacting the block, then putting the block back to the heat treatment furnace for heat treatment at the sintering temperature of the high-temperature superconductor for a certain time, and after the mixing treatment, uniformly mixing the high-temperature superconductor with the nano particles.
Further, the molar ratio of citric acid to ethylene glycol in the step (1) is in the range of 1: 2 and 1: 4, in the above range.
Further, in the step (1), a magnetic stirrer is adopted to stir the mixture uniformly.
Furthermore, the curing mold in the step (2) is a silica gel soft mold which is easy to demold and take out cured products after curing and resists the curing temperature of 130-150 ℃.
Further, the high-temperature superconductor after the mixing treatment in the step (5) is still a single-phase high-temperature superconductor.
The method of the invention for uniformly doping the nano particles in the high-temperature superconducting material skillfully utilizes the citric acid and glycol mixed organic gel to disperse the nano particles, ensures that the nano particles are not agglomerated, ensures that the size of the cured material powder of the organic gel is similar to that of the superconducting powder, thereby uniformly mixing the citric acid and the glycol mixed organic gel, keeps the temperature of the citric acid and glycol mixed organic gel at the temperature of 430-500 ℃ for a plurality of hours to completely decompose the citric acid and glycol mixed organic gel, and finally, the left is the single-phase high-temperature superconductor and the nano particles which are uniformly doped. The method has the advantages of simple and convenient operation, high efficiency, good controllability and the like.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the present invention.
Detailed Description
The present invention will now be described in detail with reference to the accompanying drawings.
Example 1
As shown in FIG. 1, a method for uniformly doping nanoparticles in a high-temperature superconductor material, the high-temperature superconductor is Bi system Bi2-xPbxSr2Ca2Cu3O10+y(Bi-2223) single-phase high-temperature superconductor, the process flow is as follows:
(1) the molar ratio of the raw materials is 1: 2, weighing citric acid and ethylene glycol, putting the ethylene glycol into a glass container, preheating the ethylene glycol in a water bath at 90 ℃, pouring the citric acid into the ethylene glycol in the water bath, stirring the mixture for 15min by using a magnetic stirrer to achieve complete mutual solubility, and then pouring a proper amount of CoFe into the mixture of the ethylene glycol and the citric acid in the water bath2O4Uniformly mixing the magnetic nanoparticles by continuously stirring for 30min, wherein the rotating speed of magnetic stirring is 900 r/min;
(2) mixing uniformly ethylene glycol, citric acid and CoFe2O4Pouring the magnetic nano-particle mixture into a silica gel soft mold, and then putting the silica gel soft mold into an air-blast drying oven to be cured for 12 hours at 130 ℃;
(3) taking out the mixture after the mixture is completely solidified, crushing the mixture by using a crusher, uniformly mixing the crushed powder with Bi-2223 single-phase high-temperature superconductor powder in a certain proportion, and pressing the mixture into blocks by using a tablet press;
(4) putting the pressed block into a heat treatment furnace, preserving heat for 3 hours at 430 ℃, and cooling to room temperature;
(5) taking out the block after heat treatment, compacting the block, putting the block back to the heat treatment furnace, preserving heat at 867 ℃ for 40h, cooling to room temperature, and performing mixing treatment to obtain the Bi-2223 single-phase high-temperature superconductor and CoFe2O4And (3) uniformly mixing the magnetic nanoparticles.
This example ingeniously uses citric acid and ethylene glycol mixed organogel to blend CoFe2O4Magnetic nanoparticles are dispersed to allow CoFe2O4Uniformly mixing the magnetic nano-particles with the Bi-2223 single-phase high-temperature superconductor after the magnetic nano-particles are not agglomerated, then preserving the temperature of the mixed organic gel of citric acid and glycol for 3 hours at 430 ℃ to completely decompose the mixed organic gel, and finally, keeping the rest of the mixed organic gel of citric acid and glycol at the temperature of 430 ℃ to obtain the magnetic nano-particlesIs a Bi-2223 single-phase high-temperature superconductor and CoFe doped uniformly2O4Magnetic nanoparticles. The method has the advantages of simple and convenient operation, high efficiency and good controllability, and can ensure that the finally obtained Bi-2223 single-phase high-temperature superconductor and CoFe2O4Magnetic nanoparticles and has achieved the advantages of uniform mixing and the like.
Example 2
As shown in FIG. 1, a method for uniformly doping nanoparticles in a high temperature superconductor material, the high temperature superconductor being yttrium YBa2Cu3O7-y(Y-123) the single-phase high-temperature superconductor comprises the following process flows:
(1) the molar ratio of the raw materials is 1: 2, weighing citric acid and ethylene glycol, putting the ethylene glycol into a glass container, preheating the ethylene glycol in a water bath at 90 ℃, pouring the citric acid into the ethylene glycol in the water bath, stirring the mixture for 15min by using a magnetic stirrer to achieve complete mutual solubility, and then pouring a proper amount of NiFe into the mixture of the ethylene glycol and the citric acid in the water bath2O4The magnetic nano particles are stirred for 30min to achieve uniform mixing, and the rotating speed of magnetic stirring is 900 r/min;
(2) mixing uniformly ethylene glycol, citric acid and NiFe2O4Pouring the magnetic nano-particle mixture into a silica gel soft mold, and then putting the silica gel soft mold into an air-blast drying oven to be cured for 12 hours at 130 ℃;
(3) taking out the mixture after the mixture is completely solidified, crushing the mixture by using a crusher, uniformly mixing the crushed powder with Y-123 single-phase high-temperature superconductor powder in a certain proportion, and pressing the mixture into blocks by using a tablet press;
(4) putting the pressed block into a heat treatment furnace, preserving heat for 3 hours at 430 ℃, and cooling to room temperature;
(5) taking out the block after heat treatment, compacting the block, putting the block back to the heat treatment furnace, keeping the temperature at 920 ℃ for 20 hours, cooling to room temperature, and mixing to obtain Y-123 single-phase high-temperature superconductor and NiFe2O4And (3) uniformly mixing the magnetic nanoparticles.
This example skillfully utilizes citric acid and ethylene glycol mixed organogel to mix NiFe2O4Dispersing magnetic nanoparticles to make NiFe2O4Uniformly mixing the magnetic nano-particles with the Y-123 single-phase high-temperature superconductor after the magnetic nano-particles are not agglomerated, then preserving the temperature of the mixed organic gel of citric acid and glycol for 3 hours at 430 ℃ to completely decompose the mixed organic gel, and finally leaving the Y-123 single-phase high-temperature superconductor and NiFe uniformly doped2O4Magnetic nanoparticles. The method has the advantages of simple and convenient operation, high efficiency and good controllability, and can ensure that the finally obtained single-phase high-temperature superconductor Y-123 and NiFe are still Y-1232O4Magnetic nanoparticles and has achieved the advantages of uniform mixing and the like.
The nano particles are doped in the high-temperature superconducting material, and the nano particles and the high-temperature superconducting powder are generally directly mixed, so that the problem that the nano particles are aggregated and the size of the nano particles is far smaller than that of the superconducting powder, so that the nano particles and the superconducting powder are mixed unevenly is not considered. When the nano particles are mixed with the high-temperature superconducting precursor powder, agglomeration occurs, and the nano particles and the high-temperature superconducting precursor powder cannot be uniformly mixed due to the fact that the nano particles and the high-temperature superconducting precursor powder are far different in size, so that the critical current density of the high-temperature superconducting composite material can be influenced. In order to obtain a high temperature superconducting composite with a high critical current density, agglomeration of nanoparticles and ununiformity of mixing must be avoided. The invention skillfully utilizes the citric acid and glycol mixed organic gel to disperse the nano particles, ensures that the nano particles are not agglomerated, ensures that the size of the organic gel condensate powder is similar to that of the superconducting powder, and can uniformly mix the citric acid and glycol mixed organic gel, keeps the temperature of the citric acid and glycol mixed organic gel at the temperature of 430-500 ℃ for a plurality of hours to completely decompose the organic gel, and finally, the left organic gel is a single-phase high-temperature superconductor and uniformly doped nano particles.
References cited in the background section are as follows:
[1]E.Hannachi,Y.Slimani,F.Ben Azzouz,A.Ekicibil.Higher intra-granular and inter-granular performances of YBCO superconductor with TiO2nano-sized particles addition,Ceramics International 44(2018)18836-18843.
[2]M.K.Ben Salem,E.Hannachi,Y.Slimani,A.Hamrita,M.Zouaoui,L.Bessais,M.Ben Salem,F.Ben Azzouz.SiO2nanoparticles addition effect on microstructure and pinning properties in YBa2Cu3Oy,Ceramics International 40(2014)4953-4962.
[3]M.Hafiz,R.Abd-Shukor.Transport critical current density of(Bi1.6Pb0.4)Sr2Ca2Cu3O 10/Ag superconductor tapes with addition of nanosized CoFe2O4,Applied Physics A 120(2015)1573-1578.
[4]N.A.A.Yahya,A.Al-Sharabi,N.R.M.Suib,W.S.Chiu,R.Abd-Shukor.Enhanced transport critical current density of(Bi,Pb)-2223/Ag superconductor tapes added with nano-sized Bi2O3,Ceramics International 42(2016)18347-18351.
in light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (5)
1. A method for uniformly doping nanoparticles in a high temperature superconducting material, comprising the steps of: (1) weighing citric acid and ethylene glycol according to a certain proportion, putting the ethylene glycol into a glass container, preheating in a constant-temperature water bath or oil bath at 70-100 ℃, then pouring the citric acid into the ethylene glycol in the water bath or oil bath, stirring for a certain time to achieve complete mutual solubility, and then pouring a proper amount of nano-particles into the mixture of the ethylene glycol and the citric acid in the water bath or oil bath, and continuously stirring for a certain time to achieve uniform mixing;
(2) pouring the uniformly mixed mixture of the glycol, the citric acid and the nano particles into a curing mold, and then placing the curing mold into a forced air drying box for curing at the temperature of 130-150 ℃, wherein the curing time is more than 8 h;
(3) taking out the mixture after the mixture is completely solidified, crushing the mixture by using a crusher, uniformly mixing the crushed powder with a certain proportion of single-phase high-temperature superconductor powder, and pressing the mixture into blocks by using a tablet press;
(4) putting the pressed block into a heat treatment furnace, preserving the heat for a plurality of hours at the temperature of 430-500 ℃, and then cooling to room temperature;
(5) and taking out the block after heat treatment, compacting the block, then putting the block back to the heat treatment furnace for heat treatment at the sintering temperature of the high-temperature superconductor for a certain time, and after the mixing treatment, uniformly mixing the high-temperature superconductor with the nano particles.
2. The method for uniformly doping nanoparticles in a high temperature superconducting material according to claim 1, wherein the molar ratio of citric acid to ethylene glycol in the step (1) is in the range of 1: 2 and 1: 4, in the above range.
3. The method for uniformly doping nanoparticles in a high temperature superconducting material according to claim 1, wherein the step (1) is performed by uniformly stirring the mixture using a magnetic stirrer.
4. The method for uniformly doping nanoparticles in a high temperature superconductor material as claimed in claim 1, wherein the curing mold in the step (2) is a soft silica gel mold which is easy to remove the cured material after curing and is resistant to the curing temperature of 130-150 ℃.
5. The method for uniformly doping nanoparticles in a high temperature superconductor material according to claim 1, wherein the high temperature superconductor after the mixing process in the step (5) is still a single phase high temperature superconductor.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211306687.2A CN115504780A (en) | 2021-01-09 | 2021-01-09 | Method for uniformly doping nano particles in high-temperature superconducting material |
| CN202110028075.0A CN112811893A (en) | 2021-01-09 | 2021-01-09 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
| PCT/CN2021/137694 WO2022148214A1 (en) | 2021-01-09 | 2021-12-14 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
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| WO2022148214A1 (en) * | 2021-01-09 | 2022-07-14 | 浙江大学台州研究院 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
| CN115072793A (en) * | 2022-07-12 | 2022-09-20 | 浙江大学台州研究院 | Preparation method of high-crystallinity antioxidant magnetic nanoparticles |
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