CN113912389A - Method for improving performance of yttrium barium copper oxide superconducting block by adding 358 barium copper oxide into solid phase block - Google Patents

Method for improving performance of yttrium barium copper oxide superconducting block by adding 358 barium copper oxide into solid phase block Download PDF

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CN113912389A
CN113912389A CN202111239004.1A CN202111239004A CN113912389A CN 113912389 A CN113912389 A CN 113912389A CN 202111239004 A CN202111239004 A CN 202111239004A CN 113912389 A CN113912389 A CN 113912389A
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李国政
吴杰
董磊
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Tianjin Normal University
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Abstract

The invention discloses a method for adding Ba into a solid phase block3Cu5O8The method for improving performance of the yttrium barium copper oxide superconducting block material comprises the steps of preparing solid phase powder, preparing liquid phase powder, pressing a compact, assembling the compact, performing high-temperature heat treatment and performing oxygen permeation treatment. By reaction at Y2O3+BaCuO2Adding Ba to the solid phase block3Cu5O8The powder melting shrinkage effect can be brought to a sample during heat treatment, the diameter expansion effect of the sample caused by the penetration of a liquid phase in a liquid phase block is counteracted, the diameter expansion rate of the sample is controlled, and the effects of reducing the internal porosity, improving the internal organization structure and improving the superconducting performance are achieved. The invention can also be used for improving the performance of other series of superconducting bulk materials such as Nd, Sm, Gd and the like.

Description

Method for improving performance of yttrium barium copper oxide superconducting block by adding 358 barium copper oxide into solid phase block
Technical Field
The invention belongs to the technical field of high-temperature copper oxide superconducting materials, and particularly relates to a method for adding Ba into a solid phase block3Cu5O8(358 barium copper oxide) method for improving performance of yttrium barium copper oxide superconducting bulk.
Background
The single domain yttrium barium copper oxide (Y-Ba-Cu-O) high temperature superconducting bulk material which is guided to grow by utilizing the top seed crystal has strong magnetic flux pinning capability and can keep high critical current density (J) under high fieldc) The material and the technology are high and new technology materials and high and new technology in the worldOne of the hotspots in the research field of surgical applications. The top seed crystal assisted melting growth (Melt growth) and infiltration growth (infiltration growth) processes are two of the most mainstream methods for preparing single-domain yttrium barium copper oxide bulk materials.
In the melt growth process, the precursor block is usually made from YBa2Cu3O7−xAnd Y2BaCuO5The precursor powder mixture is pressed. In high temperature heat treatment, YBa2Cu3O7−xThe components melt and decompose into Y2BaCuO5Solid phase and Ba3Cu5O8Liquid phase (nominal composition, essentially 3 BaCuO)2A mixture of +2 CuO). The melting decomposition of the powder is generally accompanied by a diameter shrinkage of the green body, so that the finally obtained block has a shrinkage of 10% to 20% with respect to the diameter of the green body. For the infiltration growth method, the precursor block is formed by Y2BaCuO5Precursor powder or Y2O3+BaCuO2The mixed powder is pressed and simultaneously matched with a liquid phase block rich in Ba and Cu. At high temperature, the liquid phase mass melts and penetrates the liquid phase into the precursor mass, which brings about an expansion effect to the precursor mass, and the expansion rate of the diameter is related to the mold used for the compact (whether a common mold or a split mold). When using an open-die, the expansion ratio of the sample diameter can reach 13.1% (e.g., for a precursor block diameter of 16mm, the size of the final sample can reach 18.1 mm). The expansion of the sample is usually accompanied by a low density and high porosity of the internal tissue structure, which is detrimental to the superconducting properties. Therefore, it is necessary to invent a new method for controlling the expansion rate of the diameter of the sample, improving the internal structure of the sample, and improving the superconducting properties.
Disclosure of Invention
The invention aims to provide a solid phase block through adding Ba, which can control the diameter expansion rate of a sample and improve the internal structure of the sample3Cu5O8A method for improving performance of an 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:
mixing BaCO3The mol ratio of powder to CuO powder is 1: 1, and preparing BaCuO by a solid phase reaction method2Pulverizing; then BaCuO is added2The mol ratio of the powder to the CuO powder is 3: 2 to prepare Ba3Cu5O8Pulverizing; then Y is put2O3Powder with BaCuO2Powder of Ba3Cu5O8The powder is prepared by mixing the following components in a molar ratio of 1: 1: x is uniformly mixed in proportion to be used as solid phase powder, wherein x is 0.01-0.1;
(2) preparing liquid phase powder:
will Y2O3Powder with BaCuO2The mol ratio of powder to CuO powder is 1: 10: 6 as liquid phase powder;
(3) pressing a briquette:
putting solid phase powder into a cylindrical split mold, slightly flattening by using a compression bar, then pulling out the compression bar, putting an NdBCO/YBCO/MgO film seed crystal with the size of 2mm multiplied by 2mm on the powder, then putting the compression bar into the cylindrical split mold, and then pressing the mixture into a solid phase block embedded with the film seed crystal by using a tablet press under the pressure of 200 MPa; taking liquid phase powder, putting the liquid phase powder into a cylindrical split mold, and pressing the liquid phase powder into a liquid phase block by a tablet press under the pressure of 50 MPa; then take Yb2O3Putting the powder into a cylindrical split mold, and pressing into a sheet with the thickness of about 2mm by a tablet press under the pressure of 50MPa to be used 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 for pressing the liquid phase block and the supporting block is 10mm larger than that of the die for pressing the solid phase block;
the NdBCO/YBCO/MgO film seed crystal used in the steps is provided by Ceraco ceramic coating GmbH company;
(4) assembling a billet:
the supporting block, the liquid phase block and the solid phase block are coaxially arranged on the Al from bottom to top in sequence2O3On the circular pad, 5 equal-height MgO single crystal grains are spaced; for the solid phase block, ensuring that the surface with the film seed crystal faces upwards;
(5) high-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at the heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then heating to 1045 ℃ at the heating rate of 60 ℃ per hour, and preserving the heat for 1-2 hours; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, then slowly cooling to 975 ℃ at a cooling rate of 0.2-0.4 ℃ per hour, and furnace-cooling to room temperature to obtain an YBCO single-domain bulk;
(6) oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain block material into a quartz tube furnace, and slowly cooling for 200 hours in a temperature region of 450-400 ℃ in a flowing oxygen atmosphere to obtain the yttrium barium copper oxide superconducting block material.
The invention further discloses a method for adding Ba into the solid phase block3Cu5O8The method for improving the performance of the yttrium barium copper oxide superconducting bulk is applied to the aspects of reducing the diameter expansion effect of a sample and controlling the expansion rate of the sample. The experimental results show that: at Y2O3+BaCuO2Adding Ba to the solid phase block3Cu5O8The method can bring powder melting shrinkage effect to the sample during heat treatment, offset partial sample diameter expansion effect caused by liquid phase infiltration in the liquid phase block, and control the diameter expansion rate of the sample. When 0.05 mol ratio of Ba is added into the solid phase block3Cu5O8When the sample diameter is expanded, the expansion rate of the sample diameter is 9.4 percent; when 0.1 mol ratio of Ba is added into the solid phase block3Cu5O8In this case, the expansion ratio of the sample diameter was 6.9%, which was lower than that of the solid phase cake containing no Ba added thereto3Cu5O8The diameter expansion ratio (13.1%) of the sample (b).
The invention discloses a method for adding Ba into a solid phase block3Cu5O8Compared with the prior art, the method for improving the performance of the yttrium barium copper oxide superconducting bulk material has the positive effects that:
the invention adopts an embedded film seed crystal assisted infiltration growth process to prepare the yttrium barium copper oxide superconducting block material, and the Y-axis Y-axis Y axis2O3+BaCuO2Adding Ba to the solid phase block3Cu5O8Can bring powder melting shrinkage effect to the sample during heat treatment, offset partial sample diameter expansion effect caused by liquid phase infiltration in the liquid phase block, control the diameter expansion rate of the sample and play a role in reducing internal gasPorosity, improved internal structure, and improved superconductivity. The invention can also be used for improving the performance of other series of superconducting bulk materials such as Nd, Sm, Gd and the like.
Drawings
FIG. 1 shows the addition of 0.05 mol ratio Ba prepared in example 13Cu5O8The surface topography of the yttrium barium copper oxide superconducting block;
FIG. 2 is the 0.05 molar ratio of Ba added prepared in example 13Cu5O8The magnetic suspension force curve of the yttrium barium copper oxide superconducting bulk;
FIG. 3 is the 0.1 molar ratio of Ba added prepared in example 23Cu5O8The surface topography of the yttrium barium copper oxide superconducting block;
FIG. 4 is the 0.1 molar ratio of Ba added prepared in example 23Cu5O8The magnetic suspension force curve of the yttrium barium copper oxide superconducting block.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples, but the present invention is not limited to these examples. Wherein Y is used2O3、Yb2O3、BaCO3And CuO chemical starting materials are commercially available. The NdBCO/YBCO/MgO thin film seed crystal used is supplied by Ceraco ceramic coating GmbH company.
Example 1
(1) Preparing solid phase powder:
213.8131g of BaCO are taken3Mixing powder 86.1869g CuO powder uniformly to obtain BaCO3The mol ratio of the powder to the CuO powder is 1: 1, preparing BaCuO by a solid-phase reaction method2And (3) pulverizing. 81.4516g of BaCuO is taken2The powder and 18.5484g of CuO powder are mixed evenly, namely BaCuO2The mol ratio of the powder to the CuO powder is 3: 2, preparing Ba3Cu5O8And (3) pulverizing. Get 45.0210g Y2O3Powder 46.4288g BaCuO2Powder, 8.5502g Ba3Cu5O8The powders are mixed uniformly, i.e. Y2O3Powder with BaCuO2Powder of Ba3Cu5O8The molar ratio of the powder is 1: 1: 0.05 as solid phase powder.
(2) Preparing liquid phase powder:
get 11.1721g Y2O3Powder 115.2146g BaCuO2Powder 23.6133g CuO powder is mixed evenly, namely Y2O3Powder with BaCuO2The mol ratio of the powder to the CuO powder is 1: 10: 6, as liquid phase powder.
(3) Pressing a briquette:
putting 5g of solid phase powder into a cylindrical split mold (diameter is 16 mm), slightly flattening by using a pressure lever, then pulling out the pressure lever, putting an NdBCO/YBCO/MgO film seed crystal with the size of 2mm multiplied by 2mm on the powder, then putting the pressure lever, and then pressing by using a tablet press under the pressure of 200MPa to prepare a solid phase block embedded with the film seed crystal; taking 15g of liquid phase powder, putting the powder into a cylindrical split mold (with the diameter of 26 mm), and pressing the powder into a liquid phase block by a tablet press under the pressure of 50 MPa; then 3g Yb was sampled2O3The powder was placed in a cylindrical split die (diameter 26 mm) and pressed into a sheet having a thickness of about 2mm as a support block by a tablet press under a pressure of 50 MPa. Namely, the mass ratio of the solid phase powder to the liquid phase powder is 1: and 3, the diameter of the die for pressing the liquid phase block and the supporting block is 10mm larger than that of the die for pressing the solid phase block.
(4) Assembling a billet:
the supporting block, the liquid phase block and the solid phase block are coaxially arranged on the Al from bottom to top in sequence2O3On the circular pad, 5 equal-height MgO single crystal grains are spaced; for the solid phase block, the side with the film seed crystal is ensured to be upward.
(5) High-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at the heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then the temperature is raised to 1045 ℃ at the rate of 60 ℃ per hour, and the temperature is kept for 1 hour; then the temperature is reduced to 1005 ℃ at the cooling rate of 60 ℃ per hour, and then is slowly cooled to 975 ℃ at the cooling rate of 0.4 ℃ per hour, and the temperature is cooled to room temperature along with the furnace, so as to obtain the yttrium barium copper oxide single domain bulk.
(6) Oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain block material into a quartz tube furnace, and slowly cooling for 200 hours in a temperature region of 450-400 ℃ in a flowing oxygen atmosphere to obtain the yttrium barium copper oxide superconducting block material.
Prepared addition of 0.05 mol ratio Ba3Cu5O8The yttrium barium copper oxide superconducting bulk is photographed with a camera for surface morphology, and the photograph is shown in figure 1. As can be seen from the figure, the four diameters on the surface of the sample are clear, the spontaneous nucleation phenomenon does not exist, and the sample successfully grows into a single-domain sample. The final sample had a diameter of 17.5mm and an expansion rate of about 9.4% with respect to the initial size of the briquette (16 mm), which was lower than that of the solid briquette without Ba added thereto3Cu5O8The expansion ratio of the sample (2) (13.1%).
The prepared Ba is added by 0.05 mol ratio by applying a three-dimensional magnetic field and magnetic force testing device3Cu5O8The yttrium barium copper oxide superconducting bulk is subjected to magnetic suspension force performance test at the liquid nitrogen temperature, and the result is shown in figure 2. As can be seen, the maximum maglev force of the sample is 57.84N, which is higher than that of the sample without Ba being added3Cu5O8Sample (47.16N).
Example 2
In the step (1) of preparing solid phase powder, BaCuO is prepared2Powder and Ba3Cu5O8The starting materials and preparation methods for the powders were the same as in example 1. Get 41.4748g Y2O3Powder 42.7717g BaCuO2Powder, 15.7535g Ba3Cu5O8The powders are mixed uniformly, i.e. Y2O3Powder with BaCuO2Powder of Ba3Cu5O8The molar ratio of the powder is 1: 1: 0.1, as solid phase powder.
The other steps are the same as the example 1, and the yttrium barium copper oxide superconducting bulk material is prepared.
Prepared addition of 0.1 mol ratio Ba3Cu5O8The yttrium barium copper oxide superconducting bulk is photographed with a camera for surface morphology, and the photograph is shown in FIG. 3. As can be seen from the figure, the four diameters on the surface of the sample are clear, the spontaneous nucleation phenomenon does not exist, and the sample successfully grows into a single-domain sample. The final sample had a diameter of 17.1mm and an expansion rate of about 6.9% with respect to the initial size of the briquette (16 mm), which was lower than that of the solid briquette without Ba added thereto3Cu5O8The expansion ratio of the sample (2) (13.1%).
The prepared Ba is added by 0.1 mol ratio by applying a three-dimensional magnetic field and magnetic force testing device3Cu5O8The yttrium barium copper oxide superconducting bulk is subjected to magnetic suspension force performance test at the liquid nitrogen temperature, and the result is shown in figure 4. As can be seen, the maximum maglev force of the sample is 53.44N, which is higher than that of the sample without adding Ba3Cu5O8Sample (47.16N).
Example 3
In the step (1) of preparing solid phase powder, BaCuO is prepared2Powder and Ba3Cu5O8The starting materials and preparation methods for the powders were the same as in example 1. Get 48.3266g Y2O3Powder 49.8378g BaCuO2Powder, 1.8356g Ba3Cu5O8The powders are mixed uniformly, i.e. Y2O3Powder with BaCuO2Powder of Ba3Cu5O8The molar ratio of the powder is 1: 1: 0.01, as solid phase powder.
In the step (3) of pressing the briquette, 10g of solid phase powder is put into a cylindrical split die (with the diameter of 26 mm), firstly, a pressure bar is used for slightly flattening, then the pressure bar is pulled out, a piece of NdBCO/YBCO/MgO film seed crystal with the size of about 2mm multiplied by 2mm is put on the powder, then the pressure bar is put in, and then a tablet press is used for pressing under the pressure of 200MPa to prepare a solid phase block embedded with the film seed crystal; taking 30g of liquid phase powder, putting the powder into a cylindrical split mold (the diameter is 36 mm), and pressing the powder into a liquid phase block by a tablet press under the pressure of 50 MPa; then take 6g Yb2O3The powder was placed in a cylindrical split die (diameter 36 mm) and pressed into a sheet having a thickness of about 2mm as a support block by a tablet press under a pressure of 50 MPa. Namely, the mass ratio of the solid phase powder to the liquid phase powder is 1: and 3, the diameter of the die for pressing the liquid phase block and the supporting block is 10mm larger than that of the die for pressing the solid phase block.
In the high-temperature heat treatment step (5), the assembled compact is put into a shaft furnace, the temperature is raised to 900 ℃ at the temperature rise rate of 180 ℃ per hour, and the temperature is preserved for 10 hours; then the temperature is raised to 1045 ℃ at the rate of 60 ℃ per hour, and the temperature is kept for 2 hours; then the temperature is reduced to 1005 ℃ at the cooling rate of 60 ℃ per hour, and then is slowly cooled to 975 ℃ at the cooling rate of 0.2 ℃ per hour, and the temperature is cooled to room temperature along with the furnace, so as to obtain the yttrium barium copper oxide single domain bulk.
The other steps are the same as the example 1, and the yttrium barium copper oxide superconducting bulk material is prepared.

Claims (2)

1. Adding Ba into solid phase block3Cu5O8The method for improving the performance of the yttrium barium copper oxide superconducting block is characterized by comprising the following steps of:
(1) preparing solid phase powder:
mixing BaCO3The mol ratio of powder to CuO powder is 1: 1, and preparing BaCuO by a solid phase reaction method2Pulverizing; then BaCuO is added2The mol ratio of the powder to the CuO powder is 3: 2 to prepare Ba3Cu5O8Pulverizing; then Y is put2O3Powder with BaCuO2Powder of Ba3Cu5O8The powder is prepared by mixing the following components in a molar ratio of 1: 1: x is uniformly mixed in proportion to be used as solid phase powder, wherein x is 0.01-0.1;
(2) preparing liquid phase powder:
will Y2O3Powder with BaCuO2The mol ratio of powder to CuO powder is 1: 10: 6 as liquid phase powder;
(3) pressing a briquette:
putting solid phase powder into a cylindrical split mold, slightly flattening by using a compression bar, then pulling out the compression bar, putting an NdBCO/YBCO/MgO film seed crystal with the size of 2mm multiplied by 2mm on the powder, then putting the compression bar into the cylindrical split mold, and then pressing the mixture into a solid phase block embedded with the film seed crystal by using a tablet press under the pressure of 200 MPa; taking liquid phase powder, putting the liquid phase powder into a cylindrical split mold, and pressing the liquid phase powder into a liquid phase block by a tablet press under the pressure of 50 MPa; then take Yb2O3Putting the powder into a cylindrical split mold, and pressing into a sheet with the thickness of about 2mm by a tablet press under the pressure of 50MPa to be used 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 for pressing the liquid phase block and the supporting block is 10mm larger than that of the die for pressing the solid phase block;
(4) assembling a billet:
a supporting block,The liquid phase block and the solid phase block are coaxially arranged on the Al from bottom to top in turn2O3On the circular pad, 5 equal-height MgO single crystal grains are spaced; for the solid phase block, ensuring that the surface with the film seed crystal faces upwards;
(5) high-temperature heat treatment:
putting the assembled briquettes into a pit furnace, heating to 900 ℃ at the heating rate of 180 ℃ per hour, and preserving heat for 10 hours; then heating to 1045 ℃ at the heating rate of 60 ℃ per hour, and preserving the heat for 1-2 hours; then cooling to 1005 ℃ at a cooling rate of 60 ℃ per hour, then slowly cooling to 975 ℃ at a cooling rate of 0.2-0.4 ℃ per hour, and furnace-cooling to room temperature to obtain an YBCO single-domain bulk;
(6) oxygen permeation treatment:
and (3) putting the yttrium barium copper oxide single domain block material into a quartz tube furnace, and slowly cooling for 200 hours in a temperature region of 450-400 ℃ in a flowing oxygen atmosphere to obtain the yttrium barium copper oxide superconducting block material.
2. The method of claim 1 wherein Ba is added to said solid block3Cu5O8The method for improving the performance of the yttrium barium copper oxide superconducting bulk is applied to the aspects of reducing the diameter expansion effect of a sample and controlling the expansion rate of the sample.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5232907A (en) * 1988-08-12 1993-08-03 Ngk Insulators, Ltd. Yttrium-barrium-copper oxide powder and process for manufacturing yttrium-barrium-copper oxide superconducting sintered body
CN102534787A (en) * 2012-02-28 2012-07-04 陕西师范大学 Preparation method of single domain yttrium barium copper oxide superconductor
CN103361710A (en) * 2013-07-18 2013-10-23 陕西师范大学 Method for improving preparation efficiency of single domain Y-Ba-Cu-O superconducting bulk
CN103951434A (en) * 2014-05-22 2014-07-30 天津师范大学 Method for preparing single-domain yttrium-barium-copper-oxygen superconducting block in liquid-phase source coated infiltration growing manner
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
CN105418064A (en) * 2015-11-16 2016-03-23 熊菊莲 Preparation method of nano-composite yttrium barium copper oxide bulk superconductor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5232907A (en) * 1988-08-12 1993-08-03 Ngk Insulators, Ltd. Yttrium-barrium-copper oxide powder and process for manufacturing yttrium-barrium-copper oxide superconducting sintered body
CN102534787A (en) * 2012-02-28 2012-07-04 陕西师范大学 Preparation method of single domain yttrium barium copper oxide superconductor
CN103361710A (en) * 2013-07-18 2013-10-23 陕西师范大学 Method for improving preparation efficiency of single domain Y-Ba-Cu-O superconducting bulk
CN103951434A (en) * 2014-05-22 2014-07-30 天津师范大学 Method for preparing single-domain yttrium-barium-copper-oxygen superconducting block in liquid-phase source coated infiltration growing manner
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
CN105418064A (en) * 2015-11-16 2016-03-23 熊菊莲 Preparation method of nano-composite yttrium barium copper oxide bulk superconductor

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