CN101475394B - Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing - Google Patents
Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing Download PDFInfo
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- CN101475394B CN101475394B CN2009100778638A CN200910077863A CN101475394B CN 101475394 B CN101475394 B CN 101475394B CN 2009100778638 A CN2009100778638 A CN 2009100778638A CN 200910077863 A CN200910077863 A CN 200910077863A CN 101475394 B CN101475394 B CN 101475394B
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- solder
- seed crystal
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Abstract
The invention discloses a method for preparing large-size yttrium-system block materials by using an Ag2O-added YBCO solder braze welding method, and belongs to the technical field of superconductive block material preparation. The method is to adopt a top-seeded melt-textured growth method to prepare Ag2O-added YBCO solder, adopt braze welding connecting technology to weld YBCO block materials, perform post-oxidation treatment on braze welding joints, restore the superconductivity of a YBCO braze welding sample, and obtain yttrium barium copper oxygen superconductive block materials. The invention adopts the braze welding method to prepare the YBCO superconductive block materials which have large size and complex shape and cannot be prepared by the prior method, and the YBCO superconductive block materials have similar superconductivity with single-domain block materials prepared by the top-seeded melt-textured growth method. Because developed solder compositions are similar to the chemical compositions of the prior base metal, the texture of soldering seams is similar to that of the base metal. The superconductivity of the YBCO high-temperature superconductive block materials prepared by the method can reach more than 60 percent of the prior block material.
Description
Technical field
The invention belongs to the superconductive block preparing technical field, particularly use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for large size yttrium system block material.
Background technology
Yttrium barium copper oxide YBCO (YBaCuO) superconductive block is a kind of oxide ceramic material through Peritectic Reaction generation c axle preferrel orientation crystalline structure, is a kind of high-temperature superconductor with strong flux pinning and high critical current densities.Usually adopt top seed crystal method for melting texture growing preparation,, when production large size and complicated shape YBCO bulk, run into very big difficulty owing to receive the restriction of the characteristics (very slow, per hour only growth millimeter magnitude even still less) of crystal growth.Therefore, be badly in need of the YBCO device that a kind of interconnection technique efficiently increases the size of single domain YBCO bulk or obtains the structure relative complex.The method that the present invention adopts soldering to connect realizes above-mentioned target, and the composition of superconduction solder and preparation method seem particularly important.
Summary of the invention
The purpose of this invention is to provide to use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for large size yttrium system block material.
Use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for large size yttrium system block material, it is characterized in that, adopts top seed crystal method for melting texture growing preparation to add Ag
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and this method steps is following,
(1) Ag is added in preparation
2The YBCO solder of O:
1. adopt the method for chemosynthesis prepare respectively Y-123 mutually with Y-211 mutually;
2. according to weight ratio Y-123 phase: 29～89.95%, Y-211 phase: 5～40%, Ag
2O:5～30%, CeO
2, PtO
2Or among the Pt one or more: 0.5～1%, take by weighing the material powder, uniform mixing in mixer;
3. at normal temperatures, be pressed into solder sheet or the solder piece that diameter is 10～50mm, thickness 5～20mm to the solder that mixes, pressure is 5～10MPa;
4. adopt top seed crystal method for melting texture growing preparation to add Ag
2The superconduction solder of O adopts monocrystalline SmBCO as seed crystal, together puts into sintering oven to seed crystal and solder sheet or solder piece; Seed crystal be placed on solder sheet or solder piece above; Guarantee the surperficial parallel of its ab face and solder sheet or solder piece, solder sheet or solder piece are placed on the aluminum oxide pad, between solder sheet or solder piece and aluminum oxide pad with the MgO single-chip as sealing coat; Top seed crystal method for melting texture growing preparation process: at first the speed with 100～350 ℃/h is warmed up to 990～1050 ℃; Be incubated 10～30 minutes, the speed with 50～100 ℃/h cools to 980～1020 ℃ then, and then the speed with 0.1～1 ℃/h cools to 960～970 ℃; Speed with 100～350 ℃/h cools to room temperature at last, obtains adding Ag
2The YBCO solder of O;
(2) from adding Ag
2The YBCO solder upper edge a-c of O or b-c face direction cutting thickness are that the sheet of 0.1～2mm is as solder;
(3) adopt the counterweight pressurization to fit into luggage and join,, accurately assemble two or the YBCO bulk more than two, adopt and add Ag according to the identical principle of c axle texture direction with accurate pressurization jig
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and brazing temperature is 950～980 ℃, and holding time of brazing is 10～180 minutes, and soldering atmosphere is that atmosphere or pressure are the mobile oxygen atmosphere of 5～30MPa;
(4) brazed joint being carried out rear oxidation handles; Recover the superconductivity of YBCO soldering sample; The oxygen treatment temp is 430～480 ℃, and oxygen is handled 50～80h or is that oxygen is handled 10～20h in the oxygen atmosphere of 5～30MPa at pressure in the oxygen that flows, and obtains preparing YBCO superconducting blocks.
Said Y-123 is YBa mutually
2Cu
3Ox.
Said Y-211 is Y mutually
2BaCuO
5
Beneficial effect of the present invention is: adopt method for welding to prepare the large size and the YBCO superconductive block of complicated shape that traditional method can not prepare, have the similar superconductivity of single domain bulk for preparing with top seed crystal melting texture method.Because the solder composition of exploitation and the chemical ingredients of original mother metal are closely similar, so the organizational composition of brazed seam and mother metal are also closely similar.This invention can prepare aspects such as levitated superconducting magnet train, medical treatment, military affairs needed and the large size that can not obtain through additive method at present and the YBCO superconductive device of complicated shape.The superconductivity of the YBCO high-temperature superconducting block of the present invention's preparation can reach more than 60% of original bulk.
Description of drawings
Fig. 1 is a YBCO bulk soldering assembling synoptic diagram.
Embodiment
Utilize chemical synthesis prepare Y-123 mutually with Y-211 mutually, according to certain mixed and add the Ag of certain content
2O powder and other trace elements; The method preparation of employing top seed crystal method for melting texture growing has with original mother metal and has same crystal structure, similar superconductivity, density and the approximately equalised solder of solder; Utilize method for welding to realize the connection of small size high-performance single domain YBCO bulk; Preparation brazing seam structure even, texture direction and the consistent joint of mother metal (bulk); Brazed joint is carried out rear oxidation thermal treatment fully recover (structural transformation), recover the superconductivity of joint, finally obtain large size, high performance YBCO superconductive block with the oxygen that reaches superconducting phase.Below in conjunction with embodiment and accompanying drawing the present invention is described further:
Embodiment 1
Use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for large size yttrium system block material, adopts top seed crystal method for melting texture growing preparation to add Ag
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and this method steps is following,
(1) Ag is added in preparation
2The YBCO solder of O:
1. adopt the method for chemosynthesis prepare respectively Y-123 mutually with Y-211 mutually, Y-123 is YBa mutually
2Cu
3Ox, compound method is Y
2O
3, BaCO
3, CuO mixes by nominal proportioning, 920 ℃ of sintering mix after 48 hours once more then, again 920 ℃ of sintering 48 hours; Y-211 is Y mutually
2BaCuO
5, compound method is Y
2O
3, BaCO
3, CuO mixes by nominal proportioning, 930 ℃ of sintering mix after 48 hours once more then, again 930 ℃ of sintering 48 hours;
2. according to weight ratio Y-123:69.75%, Y-211:20%, Ag
2O:10%, CeO
2: 0.25%, take by weighing the material powder, uniform mixing in mixer;
3. at normal temperatures, being pressed into diameter to the solder that mixes is 10mm, thickness 20mm solder piece, and pressure is 10MPa;
4. adopt top seed crystal method for melting texture growing preparation to add Ag
2The superconduction solder of O, (the seed crystal preparation method is that Sm-123 and Sm-211 mix according to mol ratio at 3: 1 as seed crystal to adopt monocrystalline SmBCO; The single shaft compression molding was warming up to 1100 ℃ in 3 hours, was incubated 1 hour; Speed with 200 ℃/h is cooled to 1060 ℃, is cooled to 1010 ℃ with the speed of 0.5 ℃/h, and stove is chilled to room temperature; Then machinery be cleaved into c axle orientation the fritter of 2 * 2mm to 4 * 4mm as seed crystal), together put into sintering oven (sintering oven is the high precision process furnace of six independent temperature controls) to seed crystal and solder piece, seed crystal be placed on solder sheet or solder piece above; Guarantee the surperficial parallel of its ab face and solder sheet or solder piece, the solder piece is placed on the aluminum oxide pad, between solder piece and aluminum oxide pad with the MgO single-chip as sealing coat; Top seed crystal method for melting texture growing preparation process: at first the speed with 300 ℃/h is warmed up to 1000 ℃; Be incubated 30 minutes, the speed with 100 ℃/h cools to 990 ℃ then, and then the speed with 0.2 ℃/h cools to 960 ℃; Speed with 200 ℃/h cools to room temperature at last, obtains adding Ag
2The YBCO solder of O;
(2) from adding Ag
2The YBCO solder upper edge a-c face direction cutting thickness of O is that the sheet of 1mm is as solder;
(3) adopt the counterweight pressurization to fit into luggage and join,, assemble two YBCO bulks (the YBCO bulk adopts top seed crystal method for melting texture growing preparation), adopt the interpolation Ag of above-mentioned preparation according to the identical principle of c axle texture direction with accurate pressurization jig
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and Fig. 1 is a YBCO bulk soldering assembling synoptic diagram, and brazing temperature is 965 ℃, and holding time of brazing is 120 minutes, and soldering atmosphere is air atmosphere;
(4) brazed joint is carried out rear oxidation and handle, recover the superconductivity of YBCO soldering sample, the oxygen treatment temp is 470 ℃, and oxygen is handled 67h in the oxygen that flows, and obtains preparing YBCO superconducting blocks.
The interpolation 10wt%Ag of present embodiment preparation
2The YBCO solder of O; Its fusing point is compared with the YBCO mother metal of routine preparation and has been reduced about 30～50 ℃; So between solder fusing point and YBCO mother metal fusing point is the process window of soldering, and the experiment proof adopts the superconductive block of this kind solder preparation to have the superconductivity close with the melting texture method.And can realize that n (n >=2) piece sample couples together simultaneously, so just can the very big YBCO bulk of preparation size, the superconducting characteristic of not obvious reduction bulk simultaneously.
The superconductivity of the YBCO high-temperature superconducting block of present embodiment preparation can reach more than 75% of original bulk.
Embodiment 2
Use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for large size yttrium system block material, adopts top seed crystal method for melting texture growing preparation to add Ag
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and this method steps is following,
(1) Ag is added in preparation
2The YBCO solder of O:
1. adopt the method for chemosynthesis prepare respectively Y-123 mutually with Y-211 mutually, Y-123 is YBa mutually
2Cu
3Ox, compound method is Y
2O
3, BaCO
3, CuO mixes by nominal proportioning, 920 ℃ of sintering mix after 48 hours once more then, again 920 ℃ of sintering 48 hours; Y-211 is Y mutually
2BaCuO
5, compound method is Y
2O
3, BaCO
3, CuO mixes by nominal proportioning, 930 ℃ of sintering mix after 48 hours once more then, again 930 ℃ of sintering 48 hours;
2. according to weight ratio Y-123 phase: Y-211 phase 49.5%: Ag 30%,
2O:20%, PtO
2: 0.5%, take by weighing the material powder, uniform mixing in mixer;
3. at normal temperatures, be pressed into the solder piece that diameter is 20mm, thickness 20mm to the solder that mixes, pressure is 8MPa;
4. adopt top seed crystal method for melting texture growing preparation to add Ag
2The superconduction solder of O, (the seed crystal preparation method is that Sm-123 and Sm-211 mix according to mol ratio at 3: 1 as seed crystal to adopt monocrystalline SmBCO; The single shaft compression molding was warming up to 1100 ℃ in 3 hours, was incubated 1 hour; Speed with 200 ℃/h is cooled to 1060 ℃, is cooled to 1010 ℃ with the speed of 0.5 ℃/h, and stove is chilled to room temperature; Then machinery be cleaved into c axle orientation the fritter of 2 * 2mm to 4 * 4mm as seed crystal), together put into high temperature sintering furnace to seed crystal and solder piece, seed crystal be placed on solder sheet or solder piece above; Guarantee the surperficial parallel of its ab face and solder sheet or solder piece, the solder piece is placed on the aluminum oxide pad, between solder piece and aluminum oxide pad with the MgO single-chip as sealing coat; Top seed crystal method for melting texture growing preparation process: at first the speed with 320 ℃/h is warmed up to 1020 ℃; Be incubated 20 minutes, the speed with 80 ℃/h cools to 1000 ℃ then, and then the speed with 0.3 ℃/h cools to 970 ℃; Speed with 300 ℃/h cools to room temperature at last, obtains adding Ag
2The YBCO solder of O;
(2) from adding Ag
2The YBCO solder upper edge a-c face direction cutting thickness of O is that the sheet of 1mm is as solder;
(3) adopting the counterweight pressurization to fit into luggage with accurate pressurization jig joins; According to the identical principle of c axle texture direction; Assemble three YBCO bulks (the YBCO bulk adopts top seed crystal method for melting texture growing preparation); Utilize the accurate control of the special-purpose controlled atmosphere resistance heading furnace of breadboard high precision brazing process, adopt the interpolation Ag of above-mentioned preparation
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and brazing temperature is 975 ℃, and holding time of brazing is 180 minutes, and soldering atmosphere is air atmosphere;
(4) brazed joint is carried out rear oxidation and handle, recover the superconductivity of YBCO soldering sample, the oxygen treatment temp is 455 ℃, and oxygen is handled 50h in the oxygen that flows, and obtains preparing YBCO superconducting blocks.
The superconductivity of the YBCO high-temperature superconducting block of present embodiment preparation can reach more than 73% of original bulk.
Claims (3)
1. use and add Ag
2The YBCO solder brazing legal system of O is equipped with the method for preparing YBCO superconducting blocks, it is characterized in that, adopts top seed crystal method for melting texture growing preparation to add Ag
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and this method steps is following,
(1) Ag is added in preparation
2The YBCO solder of O:
1. adopt the method for chemosynthesis prepare respectively Y-123 mutually with Y-211 mutually;
2. according to weight ratio Y-123 phase: 29～89.95%, Y-211 phase: 5～40%, Ag
2O:5～30%, CeO
2, PtO
2Or among the Pt one or more: 0.5～1%, take by weighing the material powder, uniform mixing in mixer;
3. at normal temperatures, be pressed into solder sheet or the solder piece that diameter is 10～50mm, thickness 5～20mm to the solder that mixes, pressure is 5～10MPa;
4. adopt top seed crystal method for melting texture growing preparation to add Ag
2The superconduction solder of O adopts monocrystalline SmBCO as seed crystal, together puts into sintering oven to seed crystal and solder sheet or solder piece; Seed crystal be placed on solder sheet or solder piece above; Guarantee the surperficial parallel of its ab face and solder sheet or solder piece, solder sheet or solder piece are placed on the aluminum oxide pad, between solder sheet or solder piece and aluminum oxide pad with the MgO single-chip as sealing coat; Top seed crystal method for melting texture growing preparation process: at first the speed with 100～350 ℃/h is warmed up to 990～1050 ℃; Be incubated 10～30 minutes, the speed with 50～100 ℃/h cools to 980～1020 ℃ then, and then the speed with 0.1～1 ℃/h cools to 960～970 ℃; Speed with 100～350 ℃/h cools to room temperature at last, obtains adding Ag
2The YBCO solder of O;
(2) from adding Ag
2The YBCO solder upper edge a-c of O or b-c face direction cutting thickness are that the sheet of 0.1～2mm is as solder;
(3) adopt the counterweight pressurization to fit into luggage and join,, accurately assemble two or the YBCO bulk more than two, adopt and add Ag according to the identical principle of c axle texture direction with accurate pressurization jig
2The YBCO solder of O adopts soldering to connect technology the YBCO bulk is welded, and brazing temperature is 950～980 ℃, and holding time of brazing is 10～180 minutes, and soldering atmosphere is that atmosphere or pressure are the mobile oxygen atmosphere of 5～30MPa;
(4) brazed joint being carried out rear oxidation handles; Recover the superconductivity of YBCO soldering sample; The oxygen treatment temp is 430～480 ℃, and oxygen is handled 50～80h or is that oxygen is handled 10～20h in the oxygen atmosphere of 5～30MPa at pressure in the oxygen that flows, and obtains preparing YBCO superconducting blocks.
2. Ag is added in use according to claim 1
2The YBCO solder brazing legal system of O is equipped with the method for preparing YBCO superconducting blocks, it is characterized in that, said Y-123 is YBa mutually
2Cu
3Ox.
3. Ag is added in use according to claim 1
2The YBCO solder brazing legal system of O is equipped with the method for preparing YBCO superconducting blocks, it is characterized in that, said Y-211 is Y mutually
2BaCuO
5
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| CN2009100778638A CN101475394B (en) | 2009-01-23 | 2009-01-23 | Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing |
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| CN2009100778638A CN101475394B (en) | 2009-01-23 | 2009-01-23 | Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing |
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| CN101475394B true CN101475394B (en) | 2012-07-25 |
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| 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 |
| CN105390902B (en) * | 2015-12-07 | 2019-03-01 | 清华大学深圳研究生院 | A kind of superconducting joint production method for RE, Ba and Cu oxide high temperature super conductive conductor |
| CN113443907A (en) * | 2021-04-26 | 2021-09-28 | 傲普(上海)新能源有限公司 | Material performance improvement method for high-temperature superconducting flywheel energy storage |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5591698A (en) * | 1994-12-29 | 1997-01-07 | University Of Hawaii | Low temperature (T lower than 950° C.) preparation of melt texture YBCO superconductors |
| CN1176950A (en) * | 1996-09-17 | 1998-03-25 | 中国科学院上海冶金研究所 | Method for preparing isotropic, high magnetic suspension force and high temp. superconductive shape 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 |
| CN101037339A (en) * | 2007-04-25 | 2007-09-19 | 上海大学 | Preparation method of high magnetic suspension force quasi-single domain yttrium, barium, copper and oxygen block |
| CN101066866A (en) * | 2007-05-24 | 2007-11-07 | 上海大学 | Process of preparing large quasi-single domain Y-Ba-Cu-O superconductor lump |
-
2009
- 2009-01-23 CN CN2009100778638A patent/CN101475394B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5591698A (en) * | 1994-12-29 | 1997-01-07 | University Of Hawaii | Low temperature (T lower than 950° C.) preparation of melt texture YBCO superconductors |
| CN1176950A (en) * | 1996-09-17 | 1998-03-25 | 中国科学院上海冶金研究所 | Method for preparing isotropic, high magnetic suspension force and high temp. superconductive shape 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 |
| CN101037339A (en) * | 2007-04-25 | 2007-09-19 | 上海大学 | Preparation method of high magnetic suspension force quasi-single domain yttrium, barium, copper and oxygen block |
| CN101066866A (en) * | 2007-05-24 | 2007-11-07 | 上海大学 | Process of preparing large quasi-single domain Y-Ba-Cu-O superconductor lump |
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