CN102584250A - Method for preparing REBa2Cu3Ox (REBCO) high-temperature superconducting block material - Google Patents

Method for preparing REBa2Cu3Ox (REBCO) high-temperature superconducting block material Download PDF

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CN102584250A
CN102584250A CN2012100278060A CN201210027806A CN102584250A CN 102584250 A CN102584250 A CN 102584250A CN 2012100278060 A CN2012100278060 A CN 2012100278060A CN 201210027806 A CN201210027806 A CN 201210027806A CN 102584250 A CN102584250 A CN 102584250A
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rebco
block material
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CN102584250B (en
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姚忻
颜士斌
程玲
李天宇
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Shanghai Jiaotong University
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Abstract

The invention relates to a method for preparing a REBa2Cu3Ox (REBCO) high-temperature superconducting block material, in particular to a melt texture growth (MTG) method for the REBCO high-temperature superconducting block material. The MTG method for the REBCO high-temperature superconducting block material comprises the following steps of: a) mixing raw materials; b) grinding and calcining to obtain a superconducting material rough blank; c) tabletting; d) firing; and e) cooling to obtain the REBCO high-temperature superconducting block material, namely e1) cooling to buffer temperature, and preserving heat, e2) cooling to growth temperature, and preserving heat, and e3) quenching. By the method, the technical problem that the REBCO high-temperature superconducting block material fails to grow because spontaneous nucleation is generated when temperature is reduced from the maximum temperature to the growth temperature in the conventional MTG method is solved.

Description

REBCO high-temperature superconductor block preparation methods
Technical field
The present invention relates to a kind of REBCO high-temperature superconductor block preparation methods, particularly the melting texture growing method of REBCO high-temperature superconductor block material.
Background technology
RE, Ba and Cu oxide (REBa 2Cu 3Ox, REBCO) high-temperature superconductor block material has many potential application such as aspects such as magnetic suspension force, magnetic bearing, flywheel energy storage and permanent magnets.Has bigger size, higher critical current density (Jc) and the requirement of bulk is generally at application.Therefore, the preparation of large size superconduction bulk material is the key of restriction block materials practical application.Melting texture method (MTG) is then generally believed it is a kind of RE, Ba and Cu oxide high-temperature superconductor block material preparation method that has potentiality.In preparation block materials process, often need to rise to a certain top temperature (Tmax) it is fully dissolved by the presoma that superconductive powder is pressed into, grow between fast cooling to vitellarium then.The highest temperature is being played the part of keying actions such as thawing presoma and removal impurity in this process of growth; Research shows; List considers for the influence of impurity that from the highest temperature the high highest temperature helps the elimination of impurity, and then helps the inhibition of spontaneous nucleation in the process of growth.And, promote the growth window interval that the highest temperature can enlarge rare earth barium copper oxide superconducting block effectively.But having the solute supersaturation when on the other hand, in the process of growth presoma temperature being reduced to growth temperature by the highest temperature produces.Apparently, the difference of the highest temperature and growth temperature is big more, and the solute degree of supersaturation of generation is big more, and the possibility that produces spontaneous nucleation is also just big more.When between cooling area when very big, the degree of supersaturation of generation is excessive, can directly cause the appearance of spontaneous nucleation and makes the growth failure.Therefore, seek a kind of optimization method of growing and solve that to be cooled to the excessive solute degree of supersaturation that growth temperature produces from the highest temperature be the key issue that guarantees the block materials growth.
Summary of the invention
The objective of the invention is to propose a kind of melting texture growing method of REBCO high-temperature superconductor block material; The excessive degree of supersaturation that reduction produces when the highest temperature is reduced between the vitellarium; When the highest temperature is cooled to growth temperature, produce spontaneous nucleation to solve existing melting texture growing method, cause the technical problem of REBCO high-temperature superconductor block material growth failure.
The present invention solves the problems of the technologies described above through following technical scheme, reaches the object of the invention.
REBCO high-temperature superconductor block preparation methods comprises following operation:
A) batch mixes of raw material obtains compound;
B) grinding, calcination processing obtain the superconducting material crude green body;
C) compressing tablet obtains presoma;
D) calcination;
E) cooling obtains said REBCO high-temperature superconductor block material;
It is characterized in that said operation e) cooling may further comprise the steps:
e 1) fast cooling is to cushioning temperature range, insulation;
e 2) fast cooling is to growth temperature, insulation;
e 3) quench.
The present invention realizes through following technical scheme:
The present invention introduces a buffering temperature range between the highest temperature and growth temperature, the solute supersaturation that produces in the time of can controlling cooling effectively in this interval insulation for some time is in the metastable interval it always and does not produce spontaneous nucleation.Through being controlled at the soaking time of buffering temperature range, can control the solute supersaturation effectively, and then can control the speed of growth of block materials and the generation that suppresses spontaneous nucleation.
In an embodiment of the present invention, said step e 1) described in fast cooling be with the cooling of the speed of 60-150 ℃/h.
In another embodiment of the present invention, said step e 1) described in the buffering temperature range be 1055-1085 ℃.
In another embodiment of the present invention, said step e 1) described in insulation, the time is 10-30 minute.
In another embodiment of the present invention; The said operation a) batch mixes of raw material is to get 123 phase REEs, 211 phase REE and silver elements; Percentage mix according to RE123+ (10-40) mol%RE211+15wt%Ag is even; Just, mix the RE211 of 10-40% molar percentage (with respect to RE123) according to RE123, the Ag that gets RE123 and RE211 mixed powder and 15% mass percent (with respect to RE123) again mixes.Further, said 123 phase REEs are Gd123, Nd123 or Sm123; Said 211 phase REEs are Gd211, Nd211 or Sm211.
In another embodiment of the present invention, said operation b) grind, calcination processing is that said compound is ground, place then under 890-910 ℃ the environment to carry out the calcining more than 40-50 hour; The calcining back regrinding that finishes, and then place under 890-910 ℃ the environment and carry out the calcining more than 40-50 hour.
In another embodiment of the present invention, said operation c) compressing tablet is that said superconducting material crude green body is pressed into circular pie structure.
In another embodiment of the present invention; Said operation d) calcination is meant; Add at said presoma top and to be deposited on the REBCO thin film seed on the MgO substrate, place reactors then, in 4-6 hour, be warming up to 1095-1115 ℃ and be incubated 2-3 hour.Gravel size decision 1-2 * the 1-2mm of said seed crystal.This seed crystal can buy obtain from market, for example, buys from German THEVA company.
In another embodiment of the present invention, said RE=Y, Sm, Gd or Nd.
In another embodiment of the present invention, said e 2) described in the cooling rate of cooling be 60 ℃/h-150 ℃/h, growth temperature is 1015-1055 ℃, soaking time is 40-80h.
In another embodiment of the present invention, said e 3) to quench be that rate of temperature fall with 200-300 ℃/h cools the temperature to room temperature.
The inventive method adopts the temperature program(me) melting texture growing RE, Ba and Cu oxide high-temperature superconductor block material with buffering temperature range.The spontaneous nucleation problem that the use of this new temperature program(me) produces in the time of can effectively solving and reduce to growth temperature by the highest temperature.This program can be used to prepare the REBCO high-temperature superconductor block material with superior superconductivity, for the development of block materials and use significant.
Embodiment
The melting texture growing method of REBCO high-temperature superconductor block material (RE=Y, Sm, Gd or Nd) comprises following operation:
A) batch mixes of raw material; Obtain compound; Particularly be to get 123 phase REEs, 211 phase REE and silver elements, even according to the percentage mix of RE123+ (10-40) mol%RE211+15wt%Ag, RE=Y, Sm, Gd or Nd; 123 phase REEs are Gd123, Nd123 or Sm123, and 211 phase REEs are Gd211, Nd211 or Sm211;
B) compound is ground, place then under 890-910 ℃ the environment and carry out the calcining more than 40-50 hour; The calcining back regrinding that finishes, and then place under 890-910 ℃ the environment and carry out the calcining more than 40-50 hour, the superconducting material crude green body obtained;
C) compressing tablet is pressed into circular pie structure with the superconducting material crude green body, obtains presoma;
D) add seed crystal at the top of presoma, place reactors then, in 4-6 hour, be warming up to 1095-1115 ℃ and be incubated 2-3 hour;
E) cooling obtains REBCO high-temperature superconductor block material;
Operation e) cooling may further comprise the steps:
e 1) fast cooling is to cushioning temperature range 1055-1085 ℃, is incubated 10-30 minute;
e 2) fast cooling is to growth temperature, insulation;
e 3) quench.
Embodiment 1:NdBCO/YBCO/MgO film as seed crystal melting texture growing GdBCO high-temperature superconductor block material
1), prepares burden according to the Gd123+25mol%Gd211+15wt%Ag component;
2), grind, 910 ℃ of insulations were calcined in 48 hours, ground again, 910 ℃ of insulations were calcined in 48 hours;
3), be pressed into the circular pie structure of φ 20 * 8mm, the top adds the NdBCO/YBCO/MgO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4), be warming up to 1095 ℃ in 4 hours; Be incubated 2.5 hours; With the speed fast cooling to 1055 of 60-150 ℃/h ℃, be incubated 20 minutes, again with the speed fast cooling to 1016 of 60-150 ℃/h ℃; Be incubated 70 hours, quench (rate of temperature fall with 200-300 ℃/h cools the temperature to room temperature) obtains single domain GdBCO high-temperature superconductor block material.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of φ 16 * 6mm, below liquid nitrogen temperature, have superior superconductivity, have the superconducting transition temperature (Tc) about 92K.
Embodiment 2:NdBCO/YBCO/MgO film as seed crystal melting texture growing NdBCO high-temperature superconductor block material
1, prepares burden according to the Nd123+35mol%Nd211+15wt%Ag component;
2, grind, 900 ℃ of insulations were calcined in 50 hours, ground again, and 900 ℃ of insulations were calcined in 50 hours again;
3, be pressed into the circular pie structure of φ 20 * 8mm, the top adds the NdBCO/YBCO/MgO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4, be warming up to 1115 ℃ in 5 hours; Be incubated 3 hours; With the speed fast cooling to 1085 of 60-150 ℃/h ℃, be incubated 30 minutes, again with the speed fast cooling to 1054 of 60-150 ℃/h ℃; Be incubated 60 hours, quench (rate of temperature fall with 200-300 ℃/h cools the temperature to room temperature) obtains single domain NdBCO high-temperature superconductor block material.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of φ 16 * 6mm, below liquid nitrogen temperature, have superior superconductivity, have the superconducting transition temperature (Tc) about 94K.
Embodiment 3:NdBCO/YBCO/MgO film as seed crystal melting texture growing SmBCO high-temperature superconductor block material
1, prepares burden according to the Sm123+30mol%Sm211+15wt%Ag component;
2, grind, 890 ℃ of insulations were calcined in 50 hours, ground again, adopted the same process secondary clacining;
3, be pressed into the circular pie structure of φ 30 * 10mm, the top adds the NdBCO/YBCO/MgO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4, be warming up to 1110 ℃ in 4 hours; Be incubated 2 hours; With the speed fast cooling to 1075 of 60-150 ℃/h ℃, be incubated 10 minutes, again with the speed fast cooling to 1040 of 60-150 ℃/h ℃; Be incubated 80 hours, quench (rate of temperature fall with 200-300 ℃/h cools the temperature to room temperature) obtains single domain SmBCO high-temperature superconductor block material.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of φ 24 * 8mm, below liquid nitrogen temperature, have superior superconductivity, have the superconducting transition temperature (Tc) about 93K.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area need not creative work and just can design according to the present invention make many modifications and variation.Therefore, all technician in the art all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology through the available technical scheme of logical analysis, reasoning, or a limited experiment.

Claims (10)

1.REBCO high-temperature superconductor block preparation methods comprises following operation:
A) batch mixes of raw material obtains compound;
B) grinding, calcination processing obtain the superconducting material crude green body;
C) compressing tablet obtains presoma;
D) calcination;
E) cooling obtains said REBCO high-temperature superconductor block material;
It is characterized in that said operation e) cooling may further comprise the steps:
e 1) fast cooling is to cushioning temperature range, insulation;
e 2) fast cooling is to growth temperature, insulation;
e 3) quench.
2. the method for claim 1 is characterized in that: step e 1) and e 2) described in fast cooling be with the cooling of the speed of 60-150 ℃/h.
3. the method for claim 1 is characterized in that: step e 1) described in the buffering temperature range be 1055-1085 ℃, step e 1) described in time of insulation be 10-30 minute.
4. the method for claim 1 is characterized in that: step e 2) described in growth temperature be 1015-1055 ℃, step e 2) described in time of insulation be 40-80h.
5. the method for claim 1 is characterized in that: step e 3) in quenching be that rate of temperature fall with 200-300 ℃/h cools the temperature to room temperature.
6. the method for claim 1 is characterized in that: operation a) in the batch mixes of raw material be to get 123 phase REEs, 211 phase REE and silver elements, even according to the percentage mix of RE123+ (10-40) mol%RE211+15wt%Ag.
7. method as claimed in claim 6 is characterized in that: said 123 phase REEs are Gd123, Nd123 or Sm123; Said 211 phase REEs are Gd211, Nd211 or Sm211.
8. the method for claim 1 is characterized in that: said operation b) grind, calcination processing is that said compound is ground, place then under 890-910 ℃ the environment and carry out the calcining more than 40-50 hour; The calcining back regrinding that finishes, and then place under 890-910 ℃ the environment and carry out the calcining more than 40-50 hour.
9. the method for claim 1, it is characterized in that: compressing tablet said operation c) is that said superconducting material crude green body is pressed into circular pie structure.
10. the method for claim 1; It is characterized in that: said operation d) calcination is meant; Be deposited on the REBCO thin film seed on the MgO substrate in the adding of the top of said presoma; Seed size is 1-2 * 1-2mm, places reactors then, in 4-6 hour, is warming up to 1095-1115 ℃ and be incubated 2-3 hour.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102925985A (en) * 2012-09-19 2013-02-13 上海交通大学 Method for batch growth of REBCO high temperature superconducting bulks based on two-layer silicon carbide support
CN103014861A (en) * 2012-12-27 2013-04-03 上海交通大学 Preparation method of pagoda-shaped large-size REBCO (RE-Ba-Cu-O) high-temperature superconductor block
CN103060914A (en) * 2012-12-04 2013-04-24 上海交通大学 Method for quickly growing REBCO high-temperature superconducting block by stepped slow cooling acceleration
CN103360099A (en) * 2013-07-31 2013-10-23 西北有色金属研究院 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers
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
CN108648877A (en) * 2018-03-30 2018-10-12 上海交通大学 A method of it is impregnated using organic solution and improves REBCO high-temperature superconducting thin film performances

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CN101503822A (en) * 2009-02-12 2009-08-12 上海交通大学 Preparation of rare earth barium copper oxygen superconduction bulk material under pure oxygen atmosphere
CN101723680A (en) * 2009-12-22 2010-06-09 上海大学 Preparing method of large diameter yttrium barium copper oxide superconducting single domain blocks

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102925985B (en) * 2012-09-19 2015-05-27 上海交通大学 Method for batch growth of REBCO high temperature superconducting bulks based on two-layer silicon carbide support
CN102925985A (en) * 2012-09-19 2013-02-13 上海交通大学 Method for batch growth of REBCO high temperature superconducting bulks based on two-layer silicon carbide support
CN103060914A (en) * 2012-12-04 2013-04-24 上海交通大学 Method for quickly growing REBCO high-temperature superconducting block by stepped slow cooling acceleration
CN103060914B (en) * 2012-12-04 2016-01-13 上海交通大学 Notch cuttype accelerates the method for slow cooling quick growing RE BCO high-temperature superconductor block
CN103014861A (en) * 2012-12-27 2013-04-03 上海交通大学 Preparation method of pagoda-shaped large-size REBCO (RE-Ba-Cu-O) high-temperature superconductor block
CN103014861B (en) * 2012-12-27 2016-01-13 上海交通大学 The preparation method of Pagoda-shaped large size REBCO high-temperature superconductor block
CN103360099A (en) * 2013-07-31 2013-10-23 西北有色金属研究院 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers
CN103360099B (en) * 2013-07-31 2014-08-06 西北有色金属研究院 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers
CN103614775B (en) * 2013-11-29 2015-11-25 上海交通大学 The method of the accurate single crystal of a kind of embedded seeded growth REBCO
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
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
CN103603043B (en) * 2013-11-29 2016-04-06 上海交通大学 The method of the accurate single crystal of a kind of embedded seeded growth calcium analysis YBCO
CN108648877A (en) * 2018-03-30 2018-10-12 上海交通大学 A method of it is impregnated using organic solution and improves REBCO high-temperature superconducting thin film performances

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