CN101319380B - Method for rare earth 242 phase control component for growing superconducting block material - Google Patents
Method for rare earth 242 phase control component for growing superconducting block material Download PDFInfo
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- CN101319380B CN101319380B CN2008100374184A CN200810037418A CN101319380B CN 101319380 B CN101319380 B CN 101319380B CN 2008100374184 A CN2008100374184 A CN 2008100374184A CN 200810037418 A CN200810037418 A CN 200810037418A CN 101319380 B CN101319380 B CN 101319380B
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- lre
- lre242
- powder
- hours
- lre123
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 title description 14
- 239000000843 powder Substances 0.000 claims abstract description 34
- 229910052788 barium Inorganic materials 0.000 claims abstract description 13
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 239000013590 bulk material Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract 8
- 230000012010 growth Effects 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims 2
- 239000010949 copper Substances 0.000 abstract description 10
- 239000002887 superconductor Substances 0.000 abstract description 6
- 230000007704 transition Effects 0.000 abstract description 4
- 239000000155 melt Substances 0.000 abstract description 3
- -1 rare earth barium copper oxide Chemical class 0.000 abstract 1
- 238000006467 substitution reaction Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000006104 solid solution Substances 0.000 description 7
- 238000010792 warming Methods 0.000 description 6
- FFWQPZCNBYQCBT-UHFFFAOYSA-N barium;oxocopper Chemical compound [Ba].[Cu]=O FFWQPZCNBYQCBT-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 206010021143 Hypoxia Diseases 0.000 description 2
- LGVUVWSTEGWVKM-UHFFFAOYSA-N [Cu]=O.[Ba].[Sm] Chemical compound [Cu]=O.[Ba].[Sm] LGVUVWSTEGWVKM-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000009702 powder compression Methods 0.000 description 2
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 2
- 229910002480 Cu-O Inorganic materials 0.000 description 1
- BTGZYWWSOPEHMM-UHFFFAOYSA-N [O].[Cu].[Y].[Ba] Chemical compound [O].[Cu].[Y].[Ba] BTGZYWWSOPEHMM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 208000018875 hypoxemia Diseases 0.000 description 1
- 230000001146 hypoxic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Superconductors And Manufacturing Methods Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明涉及一种稀土242相控制组分生长超导块材的方法，在前驱体中添加轻稀土242(LRE2Ba4Cu2O9，LRE＝Nd，Sm等)相粉末来控制组分，先按比例将研磨烧结后的LRE123和LRE242粉末混合研磨，压制成前驱体片，然后在其顶部放上相应的籽晶，通过熔融织构方法制备LRE-BCO块体材料。本发明采用富钡的稀土242相粉末在高温熔融状态下可以调整熔体组分，有效抑制包晶反应过程中出现的轻稀土元素和钡元素的替代情况，提高制备的轻稀土钡铜氧超导体的超导转变温度和其它性能。The invention relates to a method for growing a superconducting bulk material by controlling the composition of the rare earth 242 phase, adding light rare earth 242 (LRE 2 Ba 4 Cu 2 O 9 , LRE=Nd, Sm, etc.) phase powder to the precursor to control the composition First, the ground and sintered LRE123 and LRE242 powders were mixed and ground in proportion, pressed into a precursor sheet, and then the corresponding seed crystal was placed on top of it, and the LRE-BCO bulk material was prepared by the melt texture method. The present invention adopts the barium-rich rare earth 242 phase powder to adjust the melt composition in the high-temperature melting state, effectively suppresses the substitution of light rare earth elements and barium elements in the peritectic reaction process, and improves the prepared light rare earth barium copper oxide superconductor. superconducting transition temperature and other properties.
Description
Technical field
The present invention relates to a kind of light rare earths 242 and control the method for component growth superconducting block material mutually, particularly a kind of light rare earths 242 (LRE of the rich barium that in presoma, mixes
2Ba
4Cu
2O
9, LRE242, wherein light rare earths mainly comprises shirt and elements such as neodymium) and non-superconducting controls bath component mutually, is implemented in the method for growing high-performance light rare earths barium copper oxide superconducting block material in the air.
Background technology
Melting texture method (MTG) is generally believed it is a kind of preparation barium copper oxygen high-temperature superconductor block preparation methods that has potentiality.This class superconduction bulk material has many potential to use, as can be used for aspects such as magnetic suspension force, magnetic bearing, flywheel energy storage and permanent magnet.Therefore, at application the requirement of bulk is generally and has bigger size, higher superconducting transition temperature (T
c) and higher after the match outside critical current density (J
c).It is found that under study for action, compare with traditional yttrium barium copper oxide (YBCO) superconductor, light rare earths barium copper oxygen (LRE-BCO) superconductor, mainly comprise Nd-Ba-Cu oxygen (NdBCO) and samarium barium copper oxygen (SmBCO) superconductor, has more excellent flux pinning ability, higher critical magnetic field strength and the critical current density under High-Field.In addition, because neodymium and samarium have the high characteristic of solubleness in melt, therefore can have the higher speed of growth when this two classes superconductive block of growth, this is more favourable for preparation large volume bulk.But in melting texture growing SmBCO and the NdBCO bulk process, because the Nd atom, the Sm atom is similar with the atomic radius of Ba atom in air, substituting of rare earth atom and barium atom very easily occur, forms Sm (perhaps Nd)
1+xBa
2-xCu
3O
7Solid solution, the appearance of this Solid solution has very adverse influence for the superconducting transition temperature and the performance of block materials.In order to address this problem, there is study group to propose in process of growth, to adopt the method for low oxygen partial pressure.The environment of hypoxemia can reduce the alternative ratio of element down, can effectively reduce the formation of Solid solution.But this method required equipment is relatively more expensive, the more complicated that operates, and also under hypoxic atmosphere, the speed of growth of bulk also can be affected and reduce.Comparatively speaking, adopt the method for component control not only can reach the purpose that suppresses the Solid solution generation equally, and because growth can be carried out in air, bulk can have the speed of growth faster.Realize the component control of bulk, generally need in preparation presoma process, in the RE123 superconducting phase, mix a certain proportion of second phase with particular components ratio.By this second component (ratio that for example in SmBCO and NdBCO preparation process, needs to improve the ratio of Ba: Cu and reduce RE: Ba) of coming control growing melt during the stage with the reaction of melt at high temperature, suppress to substitute between element and purpose that Solid solution forms to reach.Compare the atmosphere control method, component control method technology is fairly simple, and operation is also than being easier to, and is less demanding to experimental situation, therefore more is applicable to the batch preparations of block materials.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of light rare earths 242 to control the method for component growth superconducting block material mutually, be implemented in the big single domain of growing fast in the air, high performance LRE-BCO superconduction bulk material.
For realizing such purpose, in technical scheme of the present invention, used a kind of LRE242 phase powder with the preparation of conventional sintering method.LRE242 second with a kind of rich barium when the preparation presoma sneaks in the LRE123 powder mutually, by the effect of LRE242 phase and melt at high temperature, adjusts the component in the process of growth melt, and what occur between LRE atom that inhibition may occur and the Ba atom substitutes.
Compared with the LRE211 non-superconducting phase that occurs in the general LRE123 superconductive block growth, LRE242 has the ratio of the ratio of higher Ba: Cu and lower LRE: Ba mutually.At high temperature LRE242 in melt can and melt react and decompose.When entering the peritectoid growth phase, certain rising appears in the ratio regular meeting of the barium element in the melt, forms the environment of a rich barium, and this moment, therefore the ratio regular meeting of LRE and Ba reduced.Light rare earths is suppressed the alternative meeting of barium element in this case, thereby can not form the LRE123 Solid solution in the Peritectic Reaction process, and what make final acquisition is exactly the LRE123 superconductive block.
Realize this class growth, the LRE123 and the LRE242 powder mixes that at first will will sinter phase according to the ratio of LRE123+ (10～30) mol%LRE242 in advance into are carried out the component batching together, after being pressed into the presoma sheet, put corresponding seed crystal material at its top, obtain the accurate single domain block materials of LRE-BCO by the heat temperature raising program.
Method concrete steps of the present invention are as follows:
1, according to LRE: Ba: Cu=1: 2: 3 and LRE: Ba: Cu=2: 4: 2 ratio is with LRE
2O
3, BaCO
3, the CuO powder mixes becomes forerunner's powder of LRE123 and LRE242.
2, after grinding two kinds of forerunner's powder evenly, LRE242 810 ℃ of left and right sides sintering 12 hours under nitrogen environment, LRE123 900 ℃ of left and right sides sintering 48 hours in air.And then grinding, sintering, this process repeats 3 times altogether, to obtain the LRE123 and the LRE242 powder of pure phase.
3, the LRE123 powder and the LRE242 powder that obtain behind the sintering is even by the mixed of LRE123+ (10～30) mol%LRE242, be pressed into the presoma sheet, and put seed crystal at the top, be used for control growing orientation.
4, the presoma sheet is placed on the MgO single crystalline substrate, whole system is put into tightness system.
5, be warming up to the following 20-50 of peritectic melting temperature ℃ of LRE-BCO in 2 hours, be incubated 1 hour; Continue heating, be warming up to above 30 ± 5 ℃ of peritectic temperature, and be incubated 1.5 hours in 2 hours.
6, temperature is reduced to the Peritectic Reaction temperature in 15 minutes, with per hour 0.5 ℃ speed cooling 20-40 hour, quenching at last makes superconduction bulk material then.
LRE242 described in the present invention (wherein LRE mainly comprises elements such as Sm, Nd) is the LRE by the rich barium of agglomerating method synthetic under the nitrogen environment
2Ba
4Cu
2O
9Phase.
The present invention adopts the component control method LRE-BCO superconductive block of growing, and a kind of new LRE242 is incorporated in the melting texture growing process of LRE123 bulk mutually.The LRE242 of rich barium can adjust bath component under high temperature fused state, the light rare earths that occurs in effective inhibition Peritectic Reaction process and the alternative case of barium element, prevent the formation of light rare earths barium copper oxygen Solid solution, improve air superconducting transition temperature and other performance of the light rare earths Ba-Cu-O superconducting body of preparation down.
Advantage of the present invention is: do not introduce other element impurity in (1) process of growth, the preparation of superconductive block is not had a negative impact; (2) need not the special atmosphere environment, technology is simple, and is easy to operate; (3) light rare earths barium copper oxygen can have the higher speed of growth under air ambient, is applicable to that therefore preparation has the high-performance high-temperature superconductor LRE-BCO block materials of big one-domain structure.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described.Following examples do not constitute limitation of the invention.
Embodiment 1: melting texture growing samarium barium copper oxygen block materials after Sm242 and the Sm123 powder mixes
1, uses BaCO
3, CuO and Sm
2O
3Powder is prepared original powder according to the component ratio of Sm123 and Sm242.
2, original powder is fully ground evenly, the Sm123 powder is 900 ℃ of left and right sides sintering 48 hours, Sm242 810 ℃ of following sintering 12 hours under nitrogen; For guaranteeing finally to obtain less Sm123 of particle and Sm242 pure phase, with powder regrinding, the sintering behind the sintering, same process is triplicate altogether.
3, the pure phase powder that obtains is prepared burden according to Sm123+ (10～30) mol%Sm242 component, powder compression ground behind the sintering is become
The circular presoma sheet of 20 * 10mm, the top is placed seed crystal and is controlled orientation.
4, the presoma sheet that presses in the step 3 is placed on the MgO single crystalline substrate, whole system is put into tightness system.
5, be warming up to 950 ℃ in 2 hours, be incubated 1 hour; Continue heating, be warming up to 1090 ℃ in 2 hours, be incubated 2 hours.
6, in 15 minutes temperature is reduced to 1060 ℃, with per hour 0.5 ℃ speed cooling 30 hours, quenching at last makes superconduction Sm123 block materials then.
Embodiment 2: melting texture growing Nd-Ba-Cu oxygen block materials after Nd242 and the Nd123 powder mixes
1, uses BaCO
3, CuO and Nd
2O
3Powder is prepared original powder according to the component ratio of Nd123 and Nd242.
2, original powder is fully ground evenly, the Nd123 powder is 900 ℃ of left and right sides sintering 48 hours, Nd242 810 ℃ of following sintering 12 hours under nitrogen; For guaranteeing finally to obtain less Nd123 of particle and Nd242 pure phase, with powder regrinding, the sintering behind the sintering, same process is triplicate altogether.
3, the pure phase powder that obtains is prepared burden according to Nd123+ (10～30) mol%Nd242 component, powder compression ground behind the sintering is become
The circular presoma sheet of 20 * 10mm, the top is placed seed crystal and is controlled orientation.
4, the presoma sheet that presses in the step 3 is placed on the MgO single crystalline substrate, whole system is put into tightness system.
5, be warming up to 950 ℃ in 2 hours, be incubated 1 hour; Continue heating, be warming up to 1130 ℃ in 2 hours, be incubated 2 hours.
6, in 15 minutes temperature is reduced to 1090 ℃, with per hour 0.5 ℃ speed cooling 30 hours, quenching at last makes superconduction Nd123 block materials then.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100374184A CN101319380B (en) | 2008-05-15 | 2008-05-15 | Method for rare earth 242 phase control component for growing superconducting block material |
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|---|---|---|---|
| CN2008100374184A CN101319380B (en) | 2008-05-15 | 2008-05-15 | Method for rare earth 242 phase control component for growing superconducting block material |
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|---|---|
| CN101319380A CN101319380A (en) | 2008-12-10 |
| CN101319380B true CN101319380B (en) | 2011-04-20 |
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| CN2008100374184A Expired - Fee Related CN101319380B (en) | 2008-05-15 | 2008-05-15 | Method for rare earth 242 phase control component for growing superconducting block material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103541011B (en) * | 2013-10-31 | 2015-12-09 | 上海交通大学 | The method of the accurate single crystal of a kind of growing RE BCO high-temperature superconductor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176950A (en) * | 1996-09-17 | 1998-03-25 | 中国科学院上海冶金研究所 | Preparation method of high temperature superconducting profile with isotropic high magnetic levitation force |
| EP1157429A1 (en) * | 1999-02-17 | 2001-11-28 | SOLVAY BARIUM STRONTIUM GmbH | Superconductive bodies made of zinc-doped copper oxide material |
| CN1446947A (en) * | 2003-01-16 | 2003-10-08 | 上海交通大学 | Method for preparing superconducting block material with thick film being as seed crystal fustion texture |
| CN1837417A (en) * | 2005-03-25 | 2006-09-27 | 北京有色金属研究总院 | Multi-seed crystal preparation method of yttrium barium copper oxygen single domain superconducting bulk |
-
2008
- 2008-05-15 CN CN2008100374184A patent/CN101319380B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176950A (en) * | 1996-09-17 | 1998-03-25 | 中国科学院上海冶金研究所 | Preparation method of high temperature superconducting profile with isotropic high magnetic levitation force |
| EP1157429A1 (en) * | 1999-02-17 | 2001-11-28 | SOLVAY BARIUM STRONTIUM GmbH | Superconductive bodies made of zinc-doped copper oxide material |
| CN1446947A (en) * | 2003-01-16 | 2003-10-08 | 上海交通大学 | Method for preparing superconducting block material with thick film being as seed crystal fustion texture |
| CN1837417A (en) * | 2005-03-25 | 2006-09-27 | 北京有色金属研究总院 | Multi-seed crystal preparation method of yttrium barium copper oxygen single domain superconducting bulk |
Non-Patent Citations (1)
| Title |
|---|
| 郑明辉等.单畴GdBaCuO块材生长工艺研究.《低温物理学报》.2003,第25卷(第S1期),425-429. * |
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| CN101319380A (en) | 2008-12-10 |
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