CN104790036B - The method that nano combined preparing YBCO superconducting blocks are grown with ytterbium base liquid phase source infiltration - Google Patents

The method that nano combined preparing YBCO superconducting blocks are grown with ytterbium base liquid phase source infiltration Download PDF

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CN104790036B
CN104790036B CN201510091849.9A CN201510091849A CN104790036B CN 104790036 B CN104790036 B CN 104790036B CN 201510091849 A CN201510091849 A CN 201510091849A CN 104790036 B CN104790036 B CN 104790036B
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李国政
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Tianjin Normal University
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Abstract

The invention discloses a kind of method that use ytterbium base liquid phase source infiltration grows nano combined preparing YBCO superconducting blocks, by preparation solid phase powder, prepare liquid phase source powder, compacting predecessor block, assembling predecessor block, infiltration and grow nano combined yttrium barium copper oxide single domain bulk, ooze oxygen process step and constitute.By using Y2O3Nano powder and BaCuO2Front axle shell, CeO2The mixture of initial powder serves as solid phase powder, by after high temperature infiltration and slow cooling growth, nano level Y being successfully introduced into preparing YBCO superconducting blocks2BaCuO5Particle, obtains superconductivity higher.Employ Yb2BaCuO5Front axle shell serves as ytterbium base liquid phase source powder compacting liquid phase source block with the mixture of the initial powder of BaO, CuO, can stably support solid phase block thereon, can be again farthest the growth supply liquid phase of yttrium, barium, copper and oxygen block.Nano combined superconduction block material present invention may also apply to prepare other series such as Nd, Sm, Gd.

Description

The method that nano combined preparing YBCO superconducting blocks are grown with ytterbium base liquid phase source infiltration
Technical field
The invention belongs to high temperature cuprate superconductor field of material technology, and in particular to one kind ytterbium base liquid phase source infiltration The method for growing nano combined preparing YBCO superconducting blocks.
Background technology
Using the single domain RE-Ba-Cu-O of top seed crystal technology guiding growth（REBCO, RE=Y, Gd, Sm, Nd etc.）High temperature surpasses Guide block material, efficiently solves " Weak link " phenomenon of grain boundaries presence in Polycrystalline and multidomain sample, can carry body higher Critical current, shows trapped flux and magnetic suspension performance higher, miniature superconducting magnet, superconducting motor, magnetic suspension bearing, The aspect such as accumulated energy flywheel and magnetic suspension train has broad application prospects.
By the RE that adulterates2BaCuO5Front axle shell is in REBa2Cu3O7−δThe tiny of Dispersed precipitate is introduced in superconduction matrix RE2BaCuO5Particle can significantly improve the flux pinning ability of REBCO superconduction block materials.Under the conditions of low field, the critical electricity of sample Current density JcWith Vf211/d211It is directly proportional（Vf211It is RE2BaCuO5Particle is in REBa2Cu3O7−δThe volume integral accounted in superconduction matrix Number, d211It is RE2BaCuO5The average grain diameter of particle）.Therefore, to obtain J higherc, it is necessary to further reduce RE2BaCuO5 The size of particle, and it is uniformly distributed it.For this people was once attempted nano level RE2BaCuO5Front axle shell is doped to REBCO and surpasses In guide block material, yet with REBa2Cu3O7−δThe growth solidification process of crystal slowly, RE2BaCuO5Particle is rich in RE3+ Ba-Cu-O liquid phases in can experience serious Ostwald roughening growth process, the RE of final sample IT2BaCuO5Particle Average grain diameter still increases to sub-micron between 1 micron, it is impossible to play maximally effective flux pinning effect.If in superconductor There is no sufficiently strong magnetic flux pinning center, its without hindrance current capacity will be restricted, so as to cause sample trapped flux and Magnetic suspension performance is relatively low, the technical indicator needed for not reaching practical application.And relatively low flux pinning force cannot also prevent height Temperature superconductive body is in liquid nitrogen temperature（77K）The flux creep produced by hot activation during work, so as to trapped flux and magnetcisuspension occur Buoyancy is with the serious problem of time decay.The presence of these problems has had a strong impact on the practical value of such material and its practical Process.
The content of the invention
The technical problems to be solved by the invention are to provide one kind to introduce nanoscale pinning center in superconduction matrix So as to method that ensure sample superconductivity, to grow with ytterbium base liquid phase source infiltration nano combined preparing YBCO superconducting blocks.
The technical scheme that solution above-mentioned technical problem is used is made up of following step：
（1）Prepare solid phase powder：
It is in molar ratio 1 by the initial powder of BaO, CuO：1 ratio is well mixed, and BaCuO is made with solid reaction process2Forerunner Powder；Again by the Y of average grain diameter 50nm2O3Nano powder and BaCuO2Front axle shell is in molar ratio 1：1 ratio mixing, while addition 0.5%~1.5%（w/w）CeO2Initial powder, is well mixed, as solid phase powder；
CeO in said ratio2Initial powder is directly appended in solid phase powder, and suppression is played in infiltration growth course Y2BaCuO5Nano-particle roughening is grown up, refines Y2BaCuO5The effect of granularity, it is ensured that nano combined preparing YBCO superconducting blocks Successful preparation；
（2）Prepare liquid phase source powder：
By Yb2O3It is in molar ratio 1 with the initial powder of BaO, CuO：1：1 ratio is well mixed, and is made of solid reaction process Yb2BaCuO5Front axle shell；Again by Yb2BaCuO5Front axle shell is in molar ratio 1 with the initial powder of BaO, CuO：9：15 ratio mixing is equal It is even, as liquid phase source powder；
（3）Compacting predecessor block：
Take solid phase powder to be put into cylindrical type mould 1, be pressed into solid phase block；Take liquid phase source powder to be put into cylindrical type mould 2, press It is made liquid phase source block；Solid phase powder wherein used is 1 with the mass ratio of liquid phase source powder：2.5~3.5, cylindrical type mould 2 it is a diameter of Than the big 10mm of cylindrical type mould 1；Yb is taken again2BaCuO5Front axle shell is put into cylindrical type mould 2, is pressed into the thin slice of thickness about 2mm, As support block；
（4）Assembling predecessor block：
Liquid phase source block, solid phase block be sequentially coaxially placed on the surface of support block from bottom to top, then by one block of neodymium barium copper Oxygen seed crystal is placed in the upper surface center of solid phase block, completes the assembling of predecessor block；
（5）Infiltration grows nano combined yttrium barium copper oxide single domain bulk：
The predecessor block that will be assembled is placed on Al2O3On pad, middle interval is then overall to put with 5 contour MgO single crystal grains Enter in shaft furnace, 800~900 DEG C are warming up to 300 DEG C per hour of heating rate, be incubated 5~15 hours；Again with per hour 60 DEG C heating rate be warming up to 1030~1040 DEG C, be incubated 0.5~1.5 hour；Then dropped with 60 DEG C per hour of rate of temperature fall Temperature to 1000~1010 DEG C, then with 0.2~0.5 DEG C per hour of rate of temperature fall slow cooling to 970~980 DEG C, with stove natural cooling To room temperature, nano combined yttrium barium copper oxide single domain bulk is obtained；
（6）Ooze oxygen treatment：
Nano combined yttrium barium copper oxide single domain bulk is put into quartz tube furnace, in the oxygen atmosphere that circulates, 450~400 DEG C warm area in slow cooling 200 hours, obtain nano combined preparing YBCO superconducting blocks.
In preparation solid phase powder step of the invention（1）In, by the Y of average grain diameter 50nm2O3Nano powder and BaCuO2Front axle shell It is in molar ratio 1：1 ratio mixing, most preferably adds 1%（w/w）CeO2Initial powder；Block step is driven before compaction（3）In, institute It is 1 with the optimum quality ratio of solid phase powder and liquid phase source powder：3；Nano combined yttrium barium copper oxide single domain bulk step is grown in infiltration（5） In, 850 DEG C most preferably are warming up to 300 DEG C per hour of heating rate, it is incubated 10 hours；Again with 60 DEG C per hour of heating rate 1035 DEG C are warming up to, 1 hour is incubated；Then 1005 DEG C are cooled to 60 DEG C per hour of rate of temperature fall, then with per hour 0.33 DEG C rate of temperature fall slow cooling to 975 DEG C, naturally cool to room temperature with stove, obtain nano combined yttrium barium copper oxide single domain bulk.
The present invention is using top seed crystal infiltration growth（TSIG）Method, by using Y2O3Nano powder and BaCuO2Front axle shell, CeO2The mixture of initial powder serves as solid phase powder, by after high temperature infiltration and slow cooling growth, in preparing YBCO superconducting blocks into Work(introduces nano level Y2BaCuO5Particle, obtains superconductivity higher.Employ Yb2BaCuO5Front axle shell and BaO, CuO The mixture of initial powder serves as ytterbium base liquid phase source powder compacting liquid phase source block, can stably support solid phase block thereon, again can be most Big degree ground is the growth supply liquid phase of yttrium, barium, copper and oxygen block.Present invention may also apply to prepare receiving for other series such as Nd, Sm, Gd Rice complex superconducting bulk.
Brief description of the drawings：
Fig. 1 is the schematic diagram of the assembling predecessor block of embodiment 1；Wherein 1 is liquid phase source block, and 2 is solid phase block, and 3 is support block, 4 is Nd-Ba-Cu oxygen seed crystal；
Fig. 2 is the surface topography map of nano combined preparing YBCO superconducting blocks prepared by embodiment 1；
Fig. 3 is the magnetic suspension force curve of nano combined preparing YBCO superconducting blocks prepared by embodiment 1；
Fig. 4 is the micro-structure diagram of nano combined preparing YBCO superconducting blocks prepared by embodiment 1.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but the invention is not restricted to these embodiments. Wherein used nanometer Y2O3（Average grain diameter 50nm）、Yb2O3、CeO2, BaO and CuO chemical raw materials are commercially available.
Embodiment 1
（1）Prepare solid phase powder：
Take 65.8415g BaO to be well mixed with the initial powder of 34.1585g CuO, i.e. the mol ratio of the initial powder of BaO and CuO is 1：1, it is made BaCuO with solid reaction process2Front axle shell；39.3842g Y are taken again2O3Nano powder（Average grain diameter 50nm）With 40.6158g BaCuO2Front axle shell mixes, while adding 0.8g CeO2Initial powder, i.e. Y2O3Nano powder and BaCuO2Front axle shell Mol ratio is 1：1, while addition 1%（w/w）CeO2Initial powder, is well mixed, as solid phase powder；
（2）Prepare liquid phase source powder：
Take 62.8564g Yb2O3It is well mixed with the initial powder of 24.4559g BaO, 12.6877g CuO, i.e. Yb2O3With The mol ratio of the initial powder of BaO, CuO is 1：1：1, it is made Yb with solid reaction process2BaCuO5Front axle shell；15.6734g is taken again Yb2BaCuO5Front axle shell is well mixed with the initial powder of 34.4977g BaO, 29.8289g CuO, i.e. Yb2BaCuO5Front axle shell with The mol ratio of the initial powder of BaO, CuO is 1：9：15, as liquid phase source powder；
（3）Compacting predecessor block：
Take 5g solid phase powder and be put into cylindrical type mould 1（Diameter 16mm）In, it is pressed into solid phase block；15g liquid phase source powder is taken to be put into Cylindrical type mould 2（Diameter 26mm）In, it is pressed into liquid phase source block；Solid phase powder i.e. used is 1 with the mass ratio of liquid phase source powder：3, circle Column type mould 2 it is a diameter of than the big 10mm of cylindrical type mould 1；3g Yb are taken again2BaCuO5Front axle shell is put into cylindrical type mould 2（Directly Footpath 26mm）In, the thin slice of thickness about 2mm is pressed into, as support block；
（4）Assembling predecessor block：
As shown in figure 1, in Fig. 1, liquid phase source block 1, solid phase block 2 are sequentially coaxially placed on into support block 3 from bottom to top Surface, then one piece of Nd-Ba-Cu oxygen seed crystal 4 is placed in the upper surface center of solid phase block 2, complete the assembling of predecessor block；
（5）Infiltration grows nano combined yttrium barium copper oxide single domain bulk：
The predecessor block that will be assembled is placed on Al2O3On pad, middle interval is then overall to put with 5 contour MgO single crystal grains Enter in shaft furnace, 850 DEG C are warming up to 300 DEG C per hour of heating rate, be incubated 10 hours；Again with 60 DEG C per hour of intensification Speed is warming up to 1035 DEG C, is incubated 1 hour；Then 1005 DEG C are cooled to 60 DEG C per hour of rate of temperature fall, then with per hour 0.33 DEG C of rate of temperature fall slow cooling naturally cools to room temperature to 975 DEG C with stove, obtains the nano combined yttrium barium copper oxide of diameter 16mm Single domain bulk；
（6）Ooze oxygen treatment：
Nano combined yttrium barium copper oxide single domain bulk is put into quartz tube furnace, in the oxygen atmosphere that circulates, 450~400 DEG C warm area in slow cooling 200 hours, obtain nano combined preparing YBCO superconducting blocks.
Prepared nano combined preparing YBCO superconducting blocks, surface topography is shot with camera, and photo is as shown in Figure 2. As seen from the figure, the footpath of sample surfaces four understands, and without spontaneous nucleation phenomenon, illustrates the superconducting block that sample successful growth is single crystal domains Material.
Magnetic suspension is carried out to the nano combined preparing YBCO superconducting blocks for preparing using three-dimensional magnetic field and magnetic force test device Power performance test, as a result as shown in Figure 3.As seen from the figure, the maximum magnetic suspension force of sample is 28.5321N, corresponding magnetic suspension force Density is 14.1907N/cm2, illustrate that sample has superior superconductivity.
In the next small chip of the marginal position cleavage of nano combined preparing YBCO superconducting blocks, using SEM Micro-Structure Analysis is carried out to it, as a result as shown in Figure 4.As seen from the figure, Dispersed precipitate a large amount of nanoscales in superconduction matrix Y2BaCuO5Particle（Average grain diameter about 50nm）, illustrate that nano level magnetic flux pinning center has been successfully introduced yttrium barium copper oxide In superconduction block material.
Embodiment 2
Preparing solid phase powder step（1）In, prepare BaCuO2Raw material and preparation method and embodiment 1 used by front axle shell It is identical, then take 39.3842g Y2O3Nano powder（Average grain diameter 50nm）With 40.6158g BaCuO2Front axle shell mixes, while addition 0.4g CeO2Initial powder, i.e. Y2O3Nano powder and BaCuO2The mol ratio of front axle shell is 1：1, while addition 0.5%（w/w）CeO2 Initial powder, is well mixed, as solid phase powder.
Block step is driven before compaction（3）In, take 5g solid phase powder and be put into cylindrical type mould 1（Diameter 16mm）In, it is pressed into solid Phase block；Take 12.5g liquid phase source powder and be put into cylindrical type mould 2（Diameter 26mm）In, it is pressed into liquid phase source block；Solid phase powder i.e. used with The mass ratio of liquid phase source powder is 1：2.5, cylindrical type mould 2 it is a diameter of than the big 10mm of cylindrical type mould 1；3g is taken again Yb2BaCuO5Front axle shell is put into cylindrical type mould 2（Diameter 26mm）In, the thin slice of thickness about 2mm is pressed into, as support block.
Nano combined yttrium barium copper oxide single domain bulk step is grown in infiltration（5）In, the predecessor block that will be assembled is placed on Al2O3 On pad, middle interval is then overall to be put into shaft furnace with 5 contour MgO single crystal grains, with 300 DEG C per hour of intensification speed Rate is warming up to 800 DEG C, is incubated 15 hours；1030 DEG C are warming up to 60 DEG C per hour of heating rate again, 1.5 hours are incubated；So 1000 DEG C are cooled to 60 DEG C per hour of rate of temperature fall afterwards, then with 0.5 DEG C per hour of rate of temperature fall slow cooling to 970 DEG C, with Stove naturally cools to room temperature, obtains the nano combined yttrium barium copper oxide single domain bulk of diameter 16mm.
Other steps are same as Example 1.Prepare nano combined preparing YBCO superconducting blocks.
Embodiment 3
Preparing solid phase powder step（1）In, prepare BaCuO2Raw material and preparation method and embodiment 1 used by front axle shell It is identical, then take 39.3842g Y2O3Nano powder（Average grain diameter 50nm）With 40.6158g BaCuO2Front axle shell mixes, while addition 1.2g CeO2Initial powder, i.e. Y2O3Nano powder and BaCuO2The mol ratio of front axle shell is 1：1, while addition 1.5%（w/w）CeO2 Initial powder, is well mixed, as solid phase powder.
Block step is driven before compaction（3）In, take 5g solid phase powder and be put into cylindrical type mould 1（Diameter 16mm）In, it is pressed into solid Phase block；Take 17.5g liquid phase source powder and be put into cylindrical type mould 2（Diameter 26mm）In, it is pressed into liquid phase source block；Solid phase powder i.e. used with The mass ratio of liquid phase source powder is 1：3.5, cylindrical type mould 2 it is a diameter of than the big 10mm of cylindrical type mould 1；3g is taken again Yb2BaCuO5Front axle shell is put into cylindrical type mould 2（Diameter 26mm）In, the thin slice of thickness about 2mm is pressed into, as support block.
Nano combined yttrium barium copper oxide single domain bulk step is grown in infiltration（5）In, the predecessor block that will be assembled is placed on Al2O3 On pad, middle interval is then overall to be put into shaft furnace with 5 contour MgO single crystal grains, with 300 DEG C per hour of intensification speed Rate is warming up to 900 DEG C, is incubated 5 hours；1040 DEG C are warming up to 60 DEG C per hour of heating rate again, 0.5 hour is incubated；Then 1010 DEG C are cooled to 60 DEG C per hour of rate of temperature fall, then with 0.25 DEG C per hour of rate of temperature fall slow cooling to 980 DEG C, with stove Room temperature is naturally cooled to, the nano combined yttrium barium copper oxide single domain bulk of diameter 16mm is obtained.
Other steps are same as Example 1.Prepare nano combined preparing YBCO superconducting blocks.
Embodiment 4
Block step is driven before compaction（3）In, take 10g solid phase powder and be put into cylindrical type mould 1（Diameter 26mm）In, it is pressed into solid Phase block；Take 30g liquid phase source powder and be put into cylindrical type mould 2（Diameter 36mm）In, it is pressed into liquid phase source block；Solid phase powder i.e. used and liquid The mass ratio of phase source powder is 1：3, cylindrical type mould 2 it is a diameter of than the big 10mm of cylindrical type mould 1；4.5g Yb are taken again2BaCuO5 Front axle shell is put into cylindrical type mould 2（Diameter 36mm）In, the thin slice of thickness about 2mm is pressed into, as support block.
Nano combined yttrium barium copper oxide single domain bulk step is grown in infiltration（5）In, the predecessor block that will be assembled is placed on Al2O3 On pad, middle interval is then overall to be put into shaft furnace with 5 contour MgO single crystal grains, with 300 DEG C per hour of intensification speed Rate is warming up to 850 DEG C, is incubated 10 hours；1035 DEG C are warming up to 60 DEG C per hour of heating rate again, 1.5 hours are incubated；So 1005 DEG C are cooled to 60 DEG C per hour of rate of temperature fall afterwards, then with 0.2 DEG C per hour of rate of temperature fall slow cooling to 975 DEG C, with Stove naturally cools to room temperature, obtains the nano combined yttrium barium copper oxide single domain bulk of diameter 26mm.
Other steps are same as Example 1.Prepare nano combined preparing YBCO superconducting blocks.
The contrast test of embodiment 5
Customary preparation methods：With Y2BaCuO5It is solid phase powder, with Y2O3With BaCuO2, CuO mixture be liquid phase source powder, use Yb2O3Compacting support block；
Preparation method of the invention：With Y2O3Nano powder and BaCuO2、CeO2Mixture be solid phase powder, with Yb2BaCuO5 Mixture with BaO, CuO is liquid phase source powder, uses Yb2BaCuO5Compacting support block；
Conclusion：
（1）The present invention can introduce nano level Y in superconduction matrix2BaCuO5Particle；
（2）Preparing YBCO superconducting blocks performance prepared by the present invention is more superior.

Claims (2)

1. a kind of method that use ytterbium base liquid phase source infiltration grows nano combined preparing YBCO superconducting blocks, it is characterised in that it is under State step composition：
（1）Prepare solid phase powder：
It is in molar ratio 1 by the initial powder of BaO, CuO：1 ratio is well mixed, and BaCuO is made with solid reaction process2Front axle shell；Again By the Y of average grain diameter 50nm2O3Nano powder and BaCuO2Front axle shell is in molar ratio 1：1 ratio mixing, while addition 0.5%~ 1.5% weight than CeO2Initial powder, is well mixed, as solid phase powder；
（2）Prepare liquid phase source powder：
By Yb2O3It is in molar ratio 1 with the initial powder of BaO, CuO：1：1 ratio is well mixed, and is made of solid reaction process Yb2BaCuO5Front axle shell；Again by Yb2BaCuO5Front axle shell is in molar ratio 1 with the initial powder of BaO, CuO：9：15 ratio mixing is equal It is even, as liquid phase source powder；
（3）Compacting predecessor block：
Take solid phase powder to be put into cylindrical type mould 1, be pressed into solid phase block；Take liquid phase source powder to be put into cylindrical type mould 2, be pressed into Liquid phase source block；Solid phase powder wherein used is 1 with the mass ratio of liquid phase source powder：2.5~3.5, a diameter of ratio circle of cylindrical type mould 2 The big 10mm of column type mould 1；Yb is taken again2BaCuO5Front axle shell is put into cylindrical type mould 2, the thin slice of thick 2mm is pressed into, as branch Bracer；
（4）Assembling predecessor block：
Liquid phase source block, solid phase block be sequentially coaxially placed on the surface of support block from bottom to top, then by one piece of Nd-Ba-Cu oxygen seed Crystalline substance is placed in the upper surface center of solid phase block, completes the assembling of predecessor block；
（5）Infiltration grows nano combined yttrium barium copper oxide single domain bulk：
The predecessor block that will be assembled is placed on Al2O3On pad, middle interval is then overall to be put into well with 5 contour MgO single crystal grains In formula stove, 800~900 DEG C are warming up to 300 DEG C per hour of heating rate, are incubated 5~15 hours；Again with 60 DEG C per hour Heating rate is warming up to 1030~1040 DEG C, is incubated 0.5~1.5 hour；Then it is cooled to 60 DEG C per hour of rate of temperature fall 1000~1010 DEG C, then room is naturally cooled to stove to 970~980 DEG C with 0.2~0.5 DEG C per hour of rate of temperature fall slow cooling Temperature, obtains nano combined yttrium barium copper oxide single domain bulk；
（6）Ooze oxygen treatment：
Nano combined yttrium barium copper oxide single domain bulk is put into quartz tube furnace, in the oxygen atmosphere that circulates, 450~400 DEG C Slow cooling 200 hours in warm area, obtain nano combined preparing YBCO superconducting blocks.
2. the method that the use ytterbium base liquid phase source infiltration described in claim 1 grows nano combined preparing YBCO superconducting blocks, it is special Levy and be：Preparing solid phase powder step（1）In, by the Y of average grain diameter 50nm2O3Nano powder and BaCuO2Front axle shell is in molar ratio It is 1：1 ratio mixing, while add 1% weight than CeO2Initial powder, is well mixed, as solid phase powder；Block is driven before compaction Step（3）In, solid phase powder used is 1 with the mass ratio of liquid phase source powder：3；Nano combined yttrium barium copper oxide single domain block is grown in infiltration Material step（5）In, the predecessor block that will be assembled is placed on Al2O3On pad, middle interval is then whole with 5 contour MgO single crystal grains Body is put into shaft furnace, and 850 DEG C are warming up to 300 DEG C per hour of heating rate, is incubated 10 hours；Again with 60 DEG C per hour Heating rate is warming up to 1035 DEG C, is incubated 1 hour；Then 1005 DEG C are cooled to 60 DEG C per hour of rate of temperature fall, then with every The rate of temperature fall slow cooling of 0.33 DEG C of hour naturally cools to room temperature to 975 DEG C with stove, obtains nano combined yttrium barium copper oxide single domain block Material.
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