CN113818071B - Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material - Google Patents

Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material Download PDF

Info

Publication number
CN113818071B
CN113818071B CN202111239164.6A CN202111239164A CN113818071B CN 113818071 B CN113818071 B CN 113818071B CN 202111239164 A CN202111239164 A CN 202111239164A CN 113818071 B CN113818071 B CN 113818071B
Authority
CN
China
Prior art keywords
powder
solid phase
copper oxide
barium copper
yttrium barium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111239164.6A
Other languages
Chinese (zh)
Other versions
CN113818071A (en
Inventor
李国政
吴杰
董磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin Normal University
Original Assignee
Tianjin Normal University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin Normal University filed Critical Tianjin Normal University
Priority to CN202111239164.6A priority Critical patent/CN113818071B/en
Publication of CN113818071A publication Critical patent/CN113818071A/en
Application granted granted Critical
Publication of CN113818071B publication Critical patent/CN113818071B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/225—Complex oxides based on rare earth copper oxides, e.g. high T-superconductors
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/45—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides
    • C04B35/4504—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides containing rare earth oxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/005—Oxydation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3215—Barium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Abstract

The invention discloses a method for preventing top seed crystal from moving in the growth process of a nano composite yttrium barium copper oxide superconducting bulk material. A small rough plastic wafer is stuck on a gasket of the die, a solid phase block with a top round pit can be obtained after the solid phase block is pressed, and the round pit is provided with a rough bottom surface, so that the movement of a film seed crystal in the round pit can be effectively prevented. The operation is very simple, but the problem that the film seed crystal moves in the heat treatment process can be effectively solved, the uncontrollability of the experiment is reduced, and the stability and the yield are improved. The invention can be popularized to the preparation process of other series superconducting blocks such as Nd, sm, gd and the like, and can also be popularized to the traditional melting growth method.

Description

Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material
Technical Field
The invention belongs to the technical field of high-temperature copper oxide superconducting materials, and particularly relates to a method for preventing top seed crystals from moving in the growth process of a nano composite yttrium barium copper oxide superconducting bulk material.
Background
Single domain yttrium barium copper oxide (Y-Ba-Cu-O, YBCO for short) superconducting bulk grown by using top seed crystal guide has strong magnetic flux pinning capability and can maintain high critical current density (J) under high field c ) It has been one of the hot spots in the international advanced technology materials and advanced technology application research fields. The top seed assisted Melt growth (Melt growth) and infiltration growth (infiltration growth) processes are the two most dominant methods for preparing single domain yttrium barium copper oxide blocks.
Neodymium barium copper oxide (Nd-Ba-Cu-O, abbreviated as NdBCO) small crystal grains and NdBCO films are two materials most commonly used as seed crystals at present. Among them, ndBCO thin films have higher melting point and thermal stability, and can more stably guide the growth of YBCO, and have received more and more attention. However, due to the characteristics of thin and light film and smooth film surface, the phenomenon that the NdBCO film moves at the top of the sample and deviates from the central position often occurs during heat treatment, which reduces the stability of the experiment. Although pressing the NdBCO film into the compact (i.e., embedded seed mode) effectively prevents movement of the seed, it often induces growth of the film substrate (typically MgO) laterally guiding the sample, resulting in a multi-domain sample that ultimately results in reduced yield of single-domain samples. Therefore, it is necessary to invent a new method to prevent the movement of the thin film seed crystal during the heat treatment of the sample, to improve the stability of the process and the yield of the single domain sample.
Disclosure of Invention
The invention aims to provide a method for preventing top seed crystal from moving in the growth process of a nano composite yttrium barium copper oxide superconducting bulk material.
The technical scheme adopted for solving the technical problems comprises the following steps:
(1) Preparing solid phase powder:
BaCO is carried out 3 The molar ratio of the powder to the CuO powder is 1:1 are mixed uniformly and prepared into BaCuO by a solid phase reaction method 2 Powder; and then Y is added 2 O 3 Nanometer powder (particle size 50-200 nm) and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:1.15:0.1, and at the same time adding 1% by weight of CeO 2 Nano powder (particle size 15-30 nm) is mixed uniformly to be used as solid phase powder;
(2) Preparing liquid phase powder:
yb is processed into 2 O 3 Powder and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:10:6, uniformly mixing the materials in proportion to obtain liquid phase powder;
(3) Pressing the briquettes:
firstly, sticking a rough plastic sheet with the diameter of 6mm and the thickness of 0.2mm on the central position of a gasket of a cylindrical split die, then taking solid phase powder, putting the solid phase powder into the cylindrical split die, then putting the gasket, ensuring that one surface with the plastic sheet faces downwards, then putting a compression bar, then pressing and forming by a tablet press under the pressure of 200MPa, and demoulding to obtain a solid phase block with a top circular pit; liquid phase powder is taken and put into a cylindrical split die and pressedPressing the tablet machine into a liquid phase block under the pressure of 50 MPa; taking Yb again 2 O 3 Placing the powder into a cylindrical split die, and pressing into a sheet with the thickness of about 2mm by using a tablet press under the pressure of 50MPa to serve as a supporting block; wherein the mass ratio of the solid phase powder to the liquid phase powder is 1:3, the diameter of the die used for pressing the liquid phase block and the supporting block is 10mm larger than that of the die used for pressing the solid phase block;
(4) Assembling the briquettes:
coaxially arranging the support block, the liquid phase block and the solid phase block on Al from bottom to top 2 O 3 On the circular gasket, 5 MgO single crystal grains with equal height are arranged at intervals; for the solid phase block, ensuring that the surface with the round pit faces upwards, and then putting a piece of NdBCO/YBCO/MgO film seed crystal with the size of about 2mm multiplied by 2mm into the round pit;
the NdBCO/YBCO/MgO film seed crystal used in the steps is provided by Ceraco ceramic coating GmbH company;
(5) And (3) carrying out high-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at a heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then heating to 1045-1105 ℃ at a heating rate of 60 ℃ per hour, and preserving heat for 1 hour; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, slowly cooling to 975 ℃ at a cooling rate of 0.2-0.33 ℃ per hour, and cooling to room temperature along with a furnace to obtain yttrium barium copper oxide single domain blocks;
(6) And (3) oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain blocks into a quartz tube furnace, and slowly cooling the yttrium barium copper oxide single domain blocks for 200 hours in a temperature region of 450-400 ℃ in an oxygen circulation atmosphere to obtain yttrium barium copper oxide superconducting blocks.
The invention further discloses application of the method for preventing the top seed crystal from moving in the growth process of the nano composite yttrium barium copper oxide superconducting bulk material in the aspects of improving the growth stability of the sample and the yield of the single-domain sample. The experimental results show that: when the film seed crystal is placed in the round pit with the rough bottom surface, the position of the film seed crystal does not move during heat treatment and is always positioned at the center of the upper surface of the sample, so that the epitaxial growth of the sample from the center to the periphery is ensured, the side surface of the film seed crystal can not contact the sample, the nucleation of the sample is prevented from being guided by the substrate of the film from the side surface, the guided growth of the sample by the bottom surface of the seed crystal is ensured, and the growth stability of the sample and the yield of single-domain samples are finally improved.
Compared with the prior art, the method for preventing the top seed crystal from moving in the growth process of the nano composite yttrium barium copper oxide superconducting bulk material has the following positive effects:
according to the invention, a small rough plastic wafer is stuck on the gasket of the die, a solid phase block with a top circular pit can be obtained after the solid phase block is pressed, and the circular pit is provided with a rough bottom surface, so that the movement of a film seed crystal in the circular pit can be effectively prevented. The operation is very simple, but the problem that the film seed crystal moves in the heat treatment process can be effectively solved, the uncontrollability of the experiment is reduced, and the stability and the yield are improved. The invention can be popularized to the preparation process of other series superconducting blocks such as Nd, sm, gd and the like, and can also be popularized to the traditional melting growth method.
Drawings
FIG. 1 is a nano Y used in example 1 2 O 3 Is a microscopic topography of (2);
FIG. 2 is a nano CeO used in example 1 2 Is a microscopic topography of (2);
FIG. 3 is a schematic diagram of a method of pressing a solid block with a top circular pit from an open-die in example 1;
FIG. 4 is a schematic diagram showing the assembly of the thin film seed crystal and the precursor compact in example 1;
FIG. 5 is a surface topography of a nanocomposite yttrium barium copper oxide superconducting bulk material prepared in example 1;
fig. 6 is a magnetic levitation force curve of the nanocomposite yttrium barium copper oxide superconducting bulk prepared in example 1.
Fig. 7 is a microstructure of the nanocomposite yttrium barium copper oxide superconducting bulk prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples, but the present invention is not limited to these examples. Wherein the used nanometer Y 2 O 3 Nano CeO 2 、Yb 2 O 3 、BaCO 3 And CuO chemical raw materials are commercially available. The NdBCO/YBCO/MgO film seed crystal used is provided by Ceraco ceramic coating GmbH company.
Example 1
(1) Preparing solid phase powder:
213.8131g BaCO was taken 3 Mixing the powder and 86.1869g CuO powder uniformly, namely BaCO 3 The molar ratio of the powder to CuO powder is 1:1, preparing BaCuO by a solid phase reaction method 2 And (5) powder. Take 45.0210g Y 2 O 3 Nanometer powder (particle size 50-200 nm), 53.3931g BaCuO 2 Mixing powder and 1.5859g CuO powder, and simultaneously adding 1g CeO 2 Nanometer powder (particle diameter 15-30 nm), and mixing uniformly to obtain Y 2 O 3 Nano powder and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:1.15:0.1, at the same time adding 1% by weight of CeO 2 Nano powder as solid phase powder. Y is Y 2 O 3 The micro morphology of the nano powder is shown in figure 1; ceO (CeO) 2 The micro-morphology of the nano-powder is shown in figure 2.
(2) Preparing liquid phase powder:
18.4721g Yb was taken 2 O 3 Powder, 109.1563g BaCuO 2 The powder and 22.3716g of CuO powder are uniformly mixed, namely Yb 2 O 3 Powder and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:10:6, as liquid phase powder.
(3) Pressing the briquettes:
firstly, sticking a rough plastic sheet with the diameter of 6mm and the thickness of 0.2mm on the central position of a gasket of a cylindrical split die (with the diameter of 16 mm), then taking 5g of solid phase powder, putting the solid phase powder into the cylindrical split die (with the diameter of 16 mm), then putting the gasket, ensuring that the surface with the plastic sheet faces downwards, putting a compression bar, then pressing and forming by a tablet press under the pressure of 200MPa, and obtaining a solid phase block with a top round pit after demoulding, wherein the process is shown in figure 3; 15g of liquid phase powder is taken and put into a cylindrical split die (diameter is 26 mm), and pressed into liquid phase blocks by a tablet press under the pressure of 50 MPa; 3g Yb was taken again 2 O 3 The powder is put into a cylindrical split die (diameter of 26 mm) and pressed into slices with the thickness of about 2mm by a tablet press under the pressure of 50MPa,as a support block. Namely, the mass ratio of the solid phase powder to the liquid phase powder is 1:3, the diameter of the die used for pressing the liquid phase block and the supporting block is 10mm larger than that of the die used for pressing the solid phase block.
(4) Assembling the briquettes:
coaxially arranging the support block, the liquid phase block and the solid phase block on Al from bottom to top 2 O 3 On the circular gasket, 5 MgO single crystal grains with equal height are arranged at intervals; for solid phase blocks, the side with round pits was guaranteed to face upward, and then a piece of NdBCO/YBCO/MgO thin film seed crystal with a size of about 2mm by 2mm was placed in the round pit, as shown in FIG. 4.
(5) And (3) carrying out high-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at a heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then heating to 1045 ℃ at a heating rate of 60 ℃ per hour, and preserving heat for 1 hour; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, then slowly cooling to 975 ℃ at a cooling rate of 0.33 ℃ per hour, and cooling to room temperature along with a furnace to obtain the yttrium barium copper oxide single domain block.
(6) And (3) oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain blocks into a quartz tube furnace, and slowly cooling for 200 hours in a temperature region of 450-400 ℃ in an oxygen circulation atmosphere to obtain the nano composite yttrium barium copper oxide superconducting blocks.
The prepared nano composite yttrium barium copper oxide superconducting bulk material grown by the guide of the thin film seed crystal in the top circular pit is used for shooting the surface morphology by a camera, and the photo is shown in figure 5. The film seed crystal is still in the circular pit, the position of the film seed crystal is not moved, the four diameters of the surface of the final sample are clear, the spontaneous nucleation phenomenon is avoided, and the film seed crystal successfully grows into a single domain sample, the diameter of the single domain sampledAbout 17.5mm.
The magnetic levitation force performance of the prepared nano composite yttrium barium copper oxide superconducting block is tested at the temperature of liquid nitrogen by using a three-dimensional magnetic field and magnetic force testing device, and the result is shown in figure 6. As can be seen from the graph, the maximum magnetic levitation force of the sample is 63.63N, and excellent superconducting performance is exhibited.
Cleavage at edge position of nano composite yttrium barium copper oxide superconducting blockThe next small wafer was subjected to microstructure analysis by a scanning electron microscope, and the result is shown in fig. 7. As can be seen, in YBa 2 Cu 3 O 7−x Y with a large number of nano-scale dimensions dispersed in the superconducting matrix 2 BaCuO 5 Particles with a particle size of tens of nanometers to hundreds of nanometers, which indicate that nanoscale magnetic flux pinning centers have been successfully introduced into yttrium barium copper oxide superconducting bulk materials.
Example 2
In the step (3) of pressing the briquettes, firstly, a rough plastic sheet with the diameter of 6mm and the thickness of 0.2mm is stuck at the central position of a gasket of a cylindrical split die (with the diameter of 26 mm), then 10g of solid phase powder is taken and put into the cylindrical split die (with the diameter of 26 mm), then the gasket is put into the gasket, the surface with the plastic sheet is ensured to face downwards, then a pressing rod is put into the gasket, then, a tablet press is used for pressing and forming under the pressure of 200MPa, and a solid phase block with a top round pit is obtained after demoulding; putting 30g of liquid phase powder into a cylindrical split die (diameter of 36 mm), and pressing into a liquid phase block by a tablet press under the pressure of 50 MPa; 6g of Yb is taken again 2 O 3 The powder was placed in a cylindrical split die (diameter 36 mm) and pressed into a sheet having a thickness of about 2mm under a pressure of 50MPa with a tablet press as a supporting block. Namely, the mass ratio of the solid phase powder to the liquid phase powder is 1:3, the diameter of the die used for pressing the liquid phase block and the supporting block is 10mm larger than that of the die used for pressing the solid phase block.
In the high-temperature heat treatment step (5), the assembled briquettes are put into a pit furnace, heated to 900 ℃ at a heating rate of 180 ℃ per hour, and kept for 10 hours; heating to 1105 ℃ at a heating rate of 60 ℃ per hour, and preserving heat for 1 hour; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, then slowly cooling to 975 ℃ at a cooling rate of 0.2 ℃ per hour, and cooling to room temperature along with a furnace to obtain the yttrium barium copper oxide single domain block.
The other steps were the same as in example 1 to obtain a yttrium barium copper oxide superconducting bulk.

Claims (2)

1. A method for preventing top seed crystal from moving in the growth process of nano composite yttrium barium copper oxide superconducting bulk material is characterized by comprising the following steps:
(1) Preparing solid phase powder:
BaCO is carried out 3 The molar ratio of the powder to the CuO powder is 1:1 are mixed uniformly and prepared into BaCuO by a solid phase reaction method 2 Powder; then the particle diameter is 50 to 200nm Y 2 O 3 Nano powder and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:1.15: mixing in 0.1 proportion, and adding CeO with particle size of 15-30 nm and 1% by weight 2 Uniformly mixing the nano powder to obtain solid phase powder;
(2) Preparing liquid phase powder:
yb is processed into 2 O 3 Powder and BaCuO 2 The molar ratio of the powder to the CuO powder is 1:10:6, uniformly mixing the materials in proportion to obtain liquid phase powder;
(3) Pressing the briquettes:
firstly, sticking a rough plastic sheet with the diameter of 6mm and the thickness of 0.2mm on the central position of a gasket of a cylindrical split die, then taking solid phase powder, putting the solid phase powder into the cylindrical split die, then putting the gasket, ensuring that one surface with the plastic sheet faces downwards, then putting a compression bar, then pressing and forming by a tablet press under the pressure of 200MPa, and demoulding to obtain a solid phase block with a top circular pit; placing liquid phase powder into a cylindrical split die, and pressing into a liquid phase block by a tablet press under the pressure of 50 MPa; taking Yb again 2 O 3 Placing the powder into a cylindrical split die, and pressing into a sheet with the thickness of 2mm by using a tablet press under the pressure of 50MPa to serve as a supporting block; wherein the mass ratio of the solid phase powder to the liquid phase powder is 1:3, the diameter of the die used for pressing the liquid phase block and the supporting block is 10mm larger than that of the die used for pressing the solid phase block;
(4) Assembling the briquettes:
coaxially arranging the support block, the liquid phase block and the solid phase block on Al from bottom to top 2 O 3 On the circular gasket, 5 MgO single crystal grains with equal height are arranged at intervals; for the solid phase block, ensuring that the surface with the round pit faces upwards, and then putting a piece of NdBCO/YBCO/MgO film seed crystal with the size of 2mm multiplied by 2mm into the round pit;
(5) And (3) carrying out high-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at a heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then heating to 1045-1105 ℃ at a heating rate of 60 ℃ per hour, and preserving heat for 1 hour; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, slowly cooling to 975 ℃ at a cooling rate of 0.2-0.33 ℃ per hour, and cooling to room temperature along with a furnace to obtain yttrium barium copper oxide single domain blocks;
(6) And (3) oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain blocks into a quartz tube furnace, and slowly cooling the yttrium barium copper oxide single domain blocks for 200 hours in a temperature region of 450-400 ℃ in an oxygen circulation atmosphere to obtain yttrium barium copper oxide superconducting blocks.
2. Use of the method for preventing movement of top seed crystals during growth of nanocomposite yttrium barium copper oxide superconducting bulk material according to claim 1 for improving sample growth stability and single domain sample yield.
CN202111239164.6A 2021-10-25 2021-10-25 Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material Active CN113818071B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111239164.6A CN113818071B (en) 2021-10-25 2021-10-25 Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111239164.6A CN113818071B (en) 2021-10-25 2021-10-25 Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material

Publications (2)

Publication Number Publication Date
CN113818071A CN113818071A (en) 2021-12-21
CN113818071B true CN113818071B (en) 2024-01-26

Family

ID=78918928

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111239164.6A Active CN113818071B (en) 2021-10-25 2021-10-25 Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material

Country Status (1)

Country Link
CN (1) CN113818071B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010038805A (en) * 1999-10-27 2001-05-15 이종훈 A fabrication technique for single crystals of high temperature superconductor by top and bottom seeding method
JP2006062897A (en) * 2004-08-25 2006-03-09 Nippon Steel Corp Superconducting oxide material and its manufacturing method
CN103603043A (en) * 2013-11-29 2014-02-26 上海交通大学 Method for growing calcium-doped YBCO quasi monocrystal from embedded seed crystal
CN103614775A (en) * 2013-11-29 2014-03-05 上海交通大学 Method for growing REBCO (Rare Earth Barium Copper Oxygen) standard single crystal in embedded seeded growth mode
CN103979951A (en) * 2014-05-22 2014-08-13 天津师范大学 Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material
CN104725035A (en) * 2015-03-02 2015-06-24 天津师范大学 Preparation method of nano composite ytrium barium copper oxide superconducting bulks
CN104790036A (en) * 2015-03-02 2015-07-22 天津师范大学 Method for infiltration growth of nanometer composite yttrium-barium-copper-oxygen superconducting block by using ytterbium-based liquid phase source
CN105236952A (en) * 2015-08-27 2016-01-13 天津师范大学 Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite
CN105418064A (en) * 2015-11-16 2016-03-23 熊菊莲 Preparation method of nano-composite yttrium barium copper oxide bulk superconductor
CN107059127A (en) * 2017-03-17 2017-08-18 陕西师范大学 A kind of bottom seed crystal infiltration growth method prepares the method for single domain rare earth barium copper oxide superconducting ring and its superconducting ring of preparation

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010038805A (en) * 1999-10-27 2001-05-15 이종훈 A fabrication technique for single crystals of high temperature superconductor by top and bottom seeding method
JP2006062897A (en) * 2004-08-25 2006-03-09 Nippon Steel Corp Superconducting oxide material and its manufacturing method
CN103603043A (en) * 2013-11-29 2014-02-26 上海交通大学 Method for growing calcium-doped YBCO quasi monocrystal from embedded seed crystal
CN103614775A (en) * 2013-11-29 2014-03-05 上海交通大学 Method for growing REBCO (Rare Earth Barium Copper Oxygen) standard single crystal in embedded seeded growth mode
CN103979951A (en) * 2014-05-22 2014-08-13 天津师范大学 Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material
CN104725035A (en) * 2015-03-02 2015-06-24 天津师范大学 Preparation method of nano composite ytrium barium copper oxide superconducting bulks
CN104790036A (en) * 2015-03-02 2015-07-22 天津师范大学 Method for infiltration growth of nanometer composite yttrium-barium-copper-oxygen superconducting block by using ytterbium-based liquid phase source
CN105236952A (en) * 2015-08-27 2016-01-13 天津师范大学 Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite
CN105418064A (en) * 2015-11-16 2016-03-23 熊菊莲 Preparation method of nano-composite yttrium barium copper oxide bulk superconductor
CN107059127A (en) * 2017-03-17 2017-08-18 陕西师范大学 A kind of bottom seed crystal infiltration growth method prepares the method for single domain rare earth barium copper oxide superconducting ring and its superconducting ring of preparation

Also Published As

Publication number Publication date
CN113818071A (en) 2021-12-21

Similar Documents

Publication Publication Date Title
CN107059127B (en) A kind of method of bottom seed crystal infiltration growth method preparation single domain rare earth barium copper oxide superconducting ring
US6569811B1 (en) Enhancement of JC in oxide superconductors
Muralidhar et al. Novel seeds applicable for mass processing of LRE-123 single-grain bulks
EP0423375B1 (en) Oxide superconductor and method of producing the same
CN113818071B (en) Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material
CN1464869A (en) Method of joining oxide superconductor and oxide superconductor joiner
Chaud et al. Fabrication and characterization of thin-wall YBCO single-domain samples
US6046139A (en) Making large, single crystal, 123 YBCO superconductors
Nariki et al. Advances in enlargement of melt-textured Gd–Ba–Cu–O superconductors
JPH05193938A (en) Oxide superconductor and production thereof
JPH1121126A (en) Production of oxide superconducting bulk
CN114057485B (en) Method for improving performance of yttrium barium copper oxide superconducting block by co-doping nano ytterbium oxide and nano bismuth oxide
JPH05201729A (en) Production of yttrium superconductor
Muralidhar et al. Novel seed for batch cold seeding production of GdBaCuO bulks
CN114182349A (en) Method for exciting superconducting performance of Ge-doped FeSeTe single crystal material by alcohol soaking method
JP2007131510A (en) Method for manufacture oxide superconductive bulky body and oxide superconductive bulky body
CN113912389B (en) Method for improving performance of yttrium barium copper oxide superconducting block by adding 358 barium copper oxide into solid phase block
Cho et al. Properties of superconducting MgB 2 single crystal grown by a modified flux method
CN114334420B (en) Method for in-situ preparation of quasi-single-domain REBCO high-temperature superconducting bulk magnetic lens
JP4690774B2 (en) Manufacturing method of oxide superconducting bulk material
JP2006062896A (en) Superconducting oxide material and its manufacturing method
Soylu et al. Composite reaction texturing of Bi-based 2212 compound
JPH11503711A (en) Method for manufacturing melt-textured volume probe based on high temperature superconductor YBa 2 lower Cu 3 lower 7 (YBCO)
JP4481701B2 (en) Manufacturing method of oxide superconducting bulk material
JP4669998B2 (en) Oxide superconductor and manufacturing method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant