CN102534787B - The preparation method of single domain yttrium barium copper oxide superconductor - Google Patents

The preparation method of single domain yttrium barium copper oxide superconductor Download PDF

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CN102534787B
CN102534787B CN201210048104.0A CN201210048104A CN102534787B CN 102534787 B CN102534787 B CN 102534787B CN 201210048104 A CN201210048104 A CN 201210048104A CN 102534787 B CN102534787 B CN 102534787B
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bacuo
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CN102534787A (en
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杨万民
王妙
李国政
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Shaanxi Normal University
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Abstract

A preparation method for single domain yttrium barium copper oxide superconductor, by preparation Y 2baCuO 5precursor powder, preparation liquid phase source powder, compacting Y 2baCuO 5pioneer's block and liquid phase block, suppress back-up block, prepare base substrate, infiltration growth single domain yttrium, barium, copper and oxygen block, ooze oxygen treatment step composition.The present invention adopts top seed crystal infiltration growth method, by adding metal oxide (Bi 2o 3powder and WO 3powder) adulterating successfully introduces second-phase nanoparticle Y 2ba 4cuBiO x/ Y 2ba 4cuMO x(M is Bi, W) forms magnetic flux pinning center, simplifies technique prepared by powder, the flux pinning ability shortening experimental period, reduce experimental cost, improve superconductive block.Have employed Y 2o 3prepare back-up block, in the slow cooling process of growth of yttrium, barium, copper and oxygen block, stably support two briquets above, stop the loss of liquid phase.The present invention can be used for preparing preparing YBCO superconducting blocks, also can be used for the high-temperature superconducting block preparing other series such as Gd, Sm, Nd, Eu.

Description

The preparation method of single domain yttrium barium copper oxide superconductor
Technical field
The invention belongs to high temperature cuprate superconductor field of material technology, be specifically related to top seed crystal infiltration growth technique and prepare oxide-doped preparing YBCO superconducting blocks.
Background technology
Single domain copper oxide high temperature superconductive block (RE-Ba-Cu-O, wherein RE is rare earth element, as Y, Gd, Nd etc.) has higher critical temperature and critical current density, and under high-intensity magnetic field, have stronger flux pinning ability.This advantage is that the application of such material in magnetic levitation technology is laid a good foundation, and particularly has a good application prospect in super-conductive magnetic suspension bearing, accumulated energy flywheel and the development such as superconduction electricmachine and generator.In the process of preparation single domain cuprate superconductor bulk, apply more technique and mainly contain two kinds, a kind of is traditional top seed crystal Melt-Textured Growth Process, and another kind is the top seed crystal infiltration growth technique grown up recent years.
Since top seed crystal infiltration growth technique is invented, receive the attention of more and more investigator, because it can solve Problems existing in conventional melt melt texture growth technology effectively, there is a large amount of pore and macrocrack, liquid phase and to run off serious, Y in the contraction of such as sample, distortion, inside 2baCuO 5spot segregation of particle etc.But there is intrinsic lattice defect in the superconductive block prepared by infiltration growth technique, e.g., the Weak link between crystal boundary, weak flux pinning ability etc., these all govern the further raising of superconductive block performance; In addition, Y in the superconductive block prepared due to top seed crystal infiltration process 2baCuO 5the particle of particle has reached 1 μm, namely reaches its minimum grain size, therefore, will improve critical current density J further cjust must introduce effective magnetic flux pinning center in YBCO superconductive block.Theoretically, only have when the size of the second phase particles introduced in superconductive block and the coherence length of YBCO close to time, just can play flux pinning effect effectively, and the coherence length of YBCO superconductor is nanometer scale, so only have the non-superconducting particle introducing nanometer scale as magnetic flux pinning center, effectively can control the oriented growth of superconductive block sheet tissue and Weak link phenomenon can be eliminated to greatest extent.Facts have proved, effectively improving in the method that material internal component and configuration aspects take, doping is one of the most practical method introducing useful effect pinning center, wherein, the Y with structure of double perovskite 2ba 4cuMO x(M is Nb, Zr, W, Ag, Mo, Bi etc.) nanoparticle is introduced in YBCO superconductor as second phase particles, effectively can improve magnetic suspension force and the critical current density J of YBCO superconductor c.But at introducing nanometer Y 2ba 4cuMO xbefore particle, the method that we must pass through repeatedly sintering and ball milling first prepares nanometer Y 2ba 4cuMO xpowder, so just substantially increases and introduces nanometer Y at YBCO superconductor 2ba 4cuMO xthe cost of particle, the present invention then efficiently solves this technical barrier.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the single domain yttrium barium copper oxide superconductor that a kind of levitation force is high, flux pinning ability is high.
Solve the problems of the technologies described above adopted technical scheme to be made up of following step:
1, solid phase precursor powder is prepared
By Y 2o 3with BaCO 3, CuO powder be in molar ratio 1: 1: 1 ratio mixing, make Y with solid state reaction 2baCuO 5powder, gets Y 2baCuO 5powder joins ball mill, adds Y 2baCuO 5the Bi of opaque amount 0.1% ~ 2% 2o 3powder or 0.1% ~ 3% WO 3powder, mixes, and is prepared into (1-x) Y 2baCuO 5+ xBi 2o 3or (1-y) Y 2baCuO 5+ yWO 3solid phase precursor powder.
0.001≤x≤0.02 in above formula, 0.001≤y≤0.03.
2, liquid phase source powder is prepared
By Y 2o 3with BaCO 3, CuO be in molar ratio 1: 4: 6 mixing, sinter YBa into solid state reaction 2cu 3o 7-δpowder, BaCO 3be 1: 1 in molar ratio with CuO, sinter BaCuO into solid state reaction 2powder, by YBa 2cu 3o 7-δpowder and CuO powder, BaCuO 2powder is to mix, as liquid phase source powder at 1: 2: 3 in molar ratio.
0≤δ≤1 in above formula.
3, solid phase pioneer's block and liquid phase block is suppressed
Get (1-x) Y 2baCuO 5+ xBi 2o 3solid phase precursor powder and liquid phase source powder, be pressed into (1-x) Y that shape same thickness is different respectively 2baCuO 5+ xBi 2o 3solid phase pioneer block and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2 ~ 1.56.
Get (1-y) Y 2baCuO 5+ yWO 3solid phase precursor powder and liquid phase source powder, be pressed into (1-y) Y that shape same thickness is different respectively 2baCuO 5+ yWO 3solid phase pioneer block and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2 ~ 1.56.
4, back-up block is suppressed
By Y 2o 3powder is pressed into and Y 2baCuO 5pioneer's block identical briquet block-shaped with liquid phase, as back-up block.
5, Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586gNd 2o 3, 32.1727gBaCO 3, 12.9687gCuO powder mixing, Nd 2o 3with BaCO 3, CuO powder mol ratio be 1: 1: 1, make Nd with solid state reaction 2baCuO 5powder.Get 20.9895g Y 2o 3, 49.2386gBaCO 3, 29.7719g CuO powder mixing, Nd 2o 3with BaCO 3, CuO powder mol ratio be 1: 4: 6, make NdBa with solid state reaction 2cu 3o 7-δpowder.By Nd 2baCuO 5powder and NdBa 2cu 3o 7-δpowder is to mix at 1: 3 according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method.
0≤δ≤1 in above formula.
6, base substrate assembling and laying method
At Al 2o 3pad upper surface to lower and on place MgO single-chip, back-up block, liquid phase block, (1-x) Y successively 2baCuO 5+ xBi 2o 3solid phase pioneer block or (1-y) Y 2baCuO 5+ yWO 3solid phase pioneer block, Nd-Ba-Cu oxygen seed crystal blocks.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 80 ~ 120 DEG C per hour, then be warming up to 1040 ~ 1045 DEG C with the temperature rise rate of 40 ~ 60 DEG C per hour, be incubated 1 ~ 2.5 hour; Be cooled to 1015 ~ 1025 DEG C with the rate of temperature fall of 60 DEG C per hour, with rate of temperature fall slow cooling to 980 ~ 990 DEG C of 0.1 ~ 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.
8, oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 440 ~ 410 DEG C, slow cooling 200 hours, obtains single domain yttrium barium copper oxide superconductor.
In preparation solid phase precursor powder step 1 of the present invention, get Y 2baCuO 5powder joins ball mill, adds Y 2baCuO 5the Bi of opaque amount 0.7% 2o 3powder, mixes, and is prepared into (1-x) Y 2baCuO 5+ xBi 2o 3solid phase precursor powder.At compacting (1-x) Y 2baCuO 5+ xBi 2o 3gu in pioneer's block and liquid phase block step 3, the optimum quality ratio of solid phase precursor powder and liquid phase source powder is 1: 1.44.In infiltration growth single domain yttrium, barium, copper and oxygen block step 6, the pioneer's block assembled is put into tube furnace, and the best is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then is warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, is incubated 2 hours; The best is cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cools to room temperature, obtain single domain yttrium barium copper oxide superconductor with stove.
In preparation solid phase precursor powder step 1 of the present invention, get Y 2baCuO 5powder joins ball mill, adds Y 2baCuO 5the WO of opaque amount 1.5% 3powder, mixes, and is prepared into (1-y) Y 2baCuO 5+ yWO 3solid phase precursor powder.At compacting (1-y) Y 2baCuO 5+ yWO 3in solid phase pioneer block and liquid phase block step 3, the optimum quality ratio of solid phase precursor powder and liquid phase source powder is 1: 1.44.In infiltration growth single domain yttrium, barium, copper and oxygen block step 6, the pioneer's block assembled is put into tube furnace, and the best is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then is warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, is incubated 2 hours; The best is cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cools to room temperature, obtain single domain yttrium barium copper oxide superconductor with stove.
Prepare in base substrate 5 of the present invention, MgO single-chip has contour 3 ~ 5.
Prepare in base substrate 5 in the present invention, back-up block of the present invention, liquid phase block, solid phase pioneer block are the right cylinder that external diameter is identical.
The present invention adopts top seed crystal infiltration growth method, by adding Bi 2o 3powder and other doped metallic oxide successfully introduce second-phase nanoparticle Y 2ba 4cuBiO x/ Y 2ba 4cuMO x(M is Bi, W) forms magnetic flux pinning center, invention not only simplifies technique prepared by powder, shortens experimental period, reduces experimental cost, and further increase the flux pinning ability of superconductive block.In the present invention, have employed Y 2o 3prepare back-up block, in the slow cooling process of growth of yttrium, barium, copper and oxygen block, stably support two briquets above, stop the loss of liquid phase.The present invention can be used for preparing preparing YBCO superconducting blocks, also can be used for the high-temperature superconducting block preparing other series such as Y, Sm, Nd, Eu.
Accompanying drawing explanation
Fig. 1 is the structural representation that in embodiment 1, in stove, sample is placed.
Fig. 2 is the surface topography map of single domain yttrium barium copper oxide superconductor prepared by embodiment 1.
Fig. 3 is the magnetic suspension force graphic representation of single domain yttrium barium copper oxide superconductor prepared by embodiment 1.
Fig. 4 is the magnetic suspension force graphic representation of single domain yttrium barium copper oxide superconductor prepared by embodiment 4.
Fig. 5 is the environmental scanning electronic microscope figure of the single domain yttrium barium copper oxide superconductor of embodiment 1
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the invention is not restricted to these embodiments.
Embodiment 1
With doped raw material Bi used 2o 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
1, preparation doping Bi 2o 3the Y of powder 2aCuO 5precursor powder
Get 67.3803g Y 2o 3, 58.88387g BaCO 3, 23.7359g CuO powder mixes, Y 2o 3with BaCO 3, CuO powder mol ratio be 1: 1: 1, make Y with solid state reaction 2baCuO 5powder.Get 100g Y 2baCuO 5powder joins ball mill, adds Y 2baCuO 5the Bi of opaque amount 0.7% 2o 3powder, mixes, and is prepared into Y 2baCuO 5precursor powder.
2, liquid phase source powder is prepared
Get 106.9064g BaCO 3, 43.0936g CuO mixes, BaCO 3be 1: 1 with the mol ratio of CuO powder, make BaCuO with solid state reaction 2powder.Get 22.6956g Y 2o 3, 79.3350g BaCO 3, 47.9695g CuO powder mixing, Y 2o 3with BaCO 3, CuO powder mol ratio be 1: 4: 6, make YBa with solid state reaction 2cu 3o 7-δpowder.By 81.4516gBaCuO 2powder, 18.5484gCuO powder, 76.7389g YBa 2cu 3o 7-δpowder mixes at ball mill, YBa 2cu 3o 7-δpowder and CuO, BaCuO 2the mol ratio of powder is 1: 2: 3, as liquid phase source powder.
0≤δ≤1 in above formula.
3, compacting doping Bi 2o 3the Y of powder 2baCuO 5pioneer's block and liquid phase block
Get 9g doping Bi 2o 3the Y of powder 2baCuO 5precursor powder, 13g liquid phase source powder, Y 2baCuO 5the mass ratio of precursor powder and liquid phase source powder is 1: 1.44, is pressed into liquid phase body and Y respectively 2baCuO 5precursor, liquid phase body and Y 2baCuO 5precursor is diameter is the right cylinder that 20mm, thickness are not identical.
4, back-up block is suppressed
Get 2.5gY 2o 3powder is pressed into the back-up block that diameter is 20mm.
5, Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586g Nd 2o 3, 32.1727g BaCO 3, 12.9687g CuO powder mixing, Nd 2o 3with BCO 3, CuO powder mol ratio be 1: 1: 1, become Nd with solid state reaction 2baCuO 5powder.Get 20.9895g Y 2o 3, 49.2386gBaCO 3, 29.7719g CuO powder mixing, Nd 2o 3with BaCO 3, CuO powder mol ratio be 1: 4: 6, make NdBa with solid state reaction 2cu 3o 7-δpowder.By Nd 2baCuO 5powder and NdBa 2cu 3o 7-δpowder is to mix at 1: 3 according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method.
0≤δ≤1 in above formula.
6, base substrate assembling and laying method
As shown in Figure 1, at Al 2o 3pad 6 upper surface to lower and on place successively 4 MgO single-chips 5, back-up block 4, liquid phase block 3, doping Bi 2o 3the Y of powder 2baCuO 5the height of pioneer's block 2, Nd-Ba-Cu oxygen seed crystal blocks Isosorbide-5-Nitrae sheet MgO single-chip 5 is identical, and Nd-Ba-Cu oxygen seed crystal blocks 1 is positioned at doping Bi 2o 3the Y of powder 2baCuO 5the central position of pioneer's block 2 upper surface.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then be warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, be incubated 2 hours; Be cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.
8, oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 410 ~ 440 DEG C, slow cooling 200 hours, is prepared into single domain yttrium barium copper oxide superconductor.
Prepared single domain yttrium barium copper oxide superconductor, take surface topography with photographic camera, Fig. 2 is shown in by surface topography photo.The Bi adulterated in a, b, c, d, e, f in figure 2o 3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%, and as seen from Figure 2, its surface all generates four symmetrical sectors of position centered by seed crystal, and has obvious cross decorative pattern.Along with Bi 2o 3the continuation of particle doping increases, and the pattern of sample there occurs trickle change, and the growth district of yttrium barium copper oxide crystal presents the trend of reduction.
To prepared single domain yttrium barium copper oxide superconductor, three-dimensional magnetic field and magnetic force test set is adopted to measure its magnetic suspension force, test result is shown in graphic representation 3, the ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconducting block top surface area (upper surface diameter is 20mm) is magnetic suspension force density, as seen from Figure 3, Bi 2o 3the magnetic suspension force of the preparing YBCO superconducting blocks prepared when being 0.7wt% of doping be 24.48N to the maximum, corresponding magnetic suspension force density is 7.80N/cm 2.
Embodiment 2
With doped raw material Bi used 2o 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At preparation doping Bi 2o 3the Y of powder 2baCuO 5in precursor powder step 1, preparation Y 2baCuO 5the raw material that powder is used and preparation method identical with embodiment 1, get 100g Y 2baCuO 5powder joins ball mill and mixes, and adds Y 2baCuO 5the Bi of opaque amount 0.1% 2o 3, mix, be prepared into doping Bi 2o 3the Y of powder 2baCuO 5precursor powder; At compacting doping Bi 2o 3the Y of powder 2baCuO 5in pioneer's block and liquid phase block step 3, get 9g and to adulterate Bi 2o 3the Y of powder 2baCuO 5precursor powder, 10.8g liquid phase source powder, doping Bi 2o 3the Y of powder 2baCuO 5the mass ratio of precursor powder and liquid phase source powder is 1: 1.2, is pressed into the doping Bi that shape same thickness is different respectively 2o 3the Y of powder 2baCuO 5precursor, liquid phase body; In infiltration growth single domain yttrium, barium, copper and oxygen block step 7, the base substrate assembled is put into tube furnace, 900 DEG C are warming up to the temperature rise rate of 80 DEG C per hour, 1045 DEG C are warming up to again with the temperature rise rate of 40 DEG C per hour, be incubated 1 hour, be cooled to 1015 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.1 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.
Embodiment 3
With doped raw material Bi used 2o 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At preparation doping Bi 2o 3the Y of powder 2baCuO 5in precursor powder step 1, preparation Y 2baCuO 5the raw material that powder is used and preparation method identical with embodiment 1, get 100gY 2baCuO 5powder joins ball mill and mixes, and adds Y 2baCuO 5the Bi of opaque amount 2% 2o 3, mix, be prepared into doping Bi 2o 3the Y of powder 2baCuO 5precursor powder; At compacting doping Bi 2o 3the Y of powder 2baCuO 5in pioneer's block and liquid phase block step 3, get 9g and to adulterate Bi 2o 3the Y of powder 2baCuO 5precursor powder, 14.04g liquid phase source powder, doping Bi 2o 3the Y of powder 2baCuO 5the mass ratio of precursor powder and liquid phase source powder is 1: 1.56, is pressed into the doping Bi that shape same thickness is different respectively 2o 3the Y of powder 2baCuO 5precursor, liquid phase body; In infiltration growth single domain yttrium, barium, copper and oxygen block step 7, the base substrate assembled is put into tube furnace, 900 DEG C are warming up to the temperature rise rate of 120 DEG C per hour, 1040 DEG C are warming up to again with the temperature rise rate of 60 DEG C per hour, be incubated 2.5 hours, be cooled to 1025 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 980 DEG C of 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.
Embodiment 4
With doped raw material WO used 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3 2baCuO 5in the step 1 of precursor powder, preparation Y 2baCuO 5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y 2baCuO 5powder joins ball mill, the Bi of interpolation 2o 3powder Y 2baCuO 5the WO of opaque amount 1.5% 3powder is replaced, and mixes, is prepared into Y 2baCuO 5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor.
Prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, test result is shown in graphic representation 4, the ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconducting block top surface area (upper surface diameter is 20mm) is magnetic suspension force density, as seen from Figure 4, WO 3the magnetic suspension force of the preparing YBCO superconducting blocks prepared when being 1.5wt% of doping be 25.76N to the maximum, corresponding magnetic suspension force density is 8.20N/cm 2.
Embodiment 5
With doped raw material WO used 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3 2baCuO 5in the step 1 of pioneer's powder, preparation Y 2baCuO 5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y 2baCuO 5powder joins ball mill, the Bi of interpolation 2o 3powder Y 2baCuO 5the WO of powder quality 0.1% 3powder is replaced, and mixes, is prepared into Y 2baCuO 5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor, and prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, and test result is shown in graphic representation 4.
Embodiment 6
With doped raw material WO used 3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3 2baCuO 5in the step 1 of precursor powder, preparation Y 2baCuO 5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y 2baCuO 5powder joins ball mill, the Bi of interpolation 2o 3powder Y 2baCuO 5the WO of opaque amount 3% 3powder is replaced, and mixes, is prepared into Y 2baCuO 5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor, and prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, and test result is shown in graphic representation 4.
In order to determine optimum material proportion of the present invention, inventors performed a large amount of laboratory study tests, various experimental conditions is as follows:
1, different oxide compounds is on the impact of single domain yttrium barium copper oxide superconductor pattern and magnetic suspension force
The preparation method of embodiment 1 is adopted to prepare single domain yttrium barium copper oxide superconductor.At preparation Y 2baCuO 5in precursor powder step 1, by analytically pure Y 2o 3(>=99.9%), BaCO 3(>=99.9%) and CuO (>=99.9%) massage that, than the ratio mixing being 1: 1: 1, makes Y with solid state reaction 2baCuO 5powder.Get Y 2baCuO 5powder joins ball mill, and add metal oxide, oxide compound selects Bi 2o 3powder, WO 3any one in powder, mixes, is prepared into Y 2baCuO 5precursor powder, Bi 2o 3powder, WO 3the consumption of powder is as follows:
(1) Y is added 2baCuO 5the Bi of opaque amount 0.1%, 0.3%, 0.5%, 0.7%, 0.9%, 2% 2o 3powder, mixes, and is prepared into Y 2baCuO 5precursor powder.Other steps are identical with embodiment 1, and being prepared into diameter is 20mm single domain yttrium barium copper oxide superconductor, adopt three-dimensional magnetic field and magnetic force test set to test magnetic suspension force respectively to prepared single domain yttrium barium copper oxide superconductor.Test result is in table 1 and Fig. 3, and in figure 3, curve a is 0.1wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve b is 0.3wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve c is 0.5wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve d is 0.7wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve e is 0.9wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve f is 2.0wt%Bi 2o 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping.Fig. 2 is seen, the Bi adulterated in a, b, c, d, e, f in figure with the take pictures surface topography map of single domain yttrium barium copper oxide superconductor of photographic camera 2o 3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%.Analyze by the structure of environmental scanning electronic microscope to single domain yttrium barium copper oxide superconductor, stereoscan photograph is shown in Fig. 5, the Bi adulterated in a, b, c, d, e, f in Fig. 5 2o 3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%.
The magnetic suspension force test data of single domain yttrium barium copper oxide superconductor prepared by table 1 embodiment 1
As seen from Figure 2, the surface of preparing YBCO superconducting blocks has all grown up to four symmetrical sectors of position centered by Nd-Ba-Cu oxygen seed crystal, and has obvious cross decorative pattern.Along with Bi 2o 3the increase of doping, the surface topography of preparing YBCO superconducting blocks there occurs trickle change, and the growth district of preparing YBCO superconducting blocks presents the trend of reduction.From table 1 and Fig. 3, Bi 2o 3the magnetic suspension force that particle doping is followed successively by the preparing YBCO superconducting blocks of 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt% be respectively 6.84N, 18.48,21.72N, 24.48N, 12.42N, 5.76N, as can be seen here, work as Bi 2o 3when particle doping is 0.7wt%, the magnetic suspension force of preparing YBCO superconducting blocks is up to 24.48N.As seen from Figure 5, be distributed with two kinds of particles in yttrium barium copper oxide superconduction matrix, wherein larger canescence particle is Y 2baCuO 5phase, it is evenly distributed in the middle of yttrium barium copper oxide superconduction matrix, and the size of particle is 1.0 μm ~ 5.0 μm; The particle of another less point-like is by Bi 2o 3particle reacts the nanometer Y of generation under semi-melting state 2ba 4cuMO xparticle, the size of particle, between 80nm ~ 160nm, compares Y 2baCuO 5particle is little one to two orders of magnitude, relative to Y 2baCuO 5particle, Y 2ba 4cuBiO xbe on good terms and play flux pinning effect better, thus effectively can improve flux pinning ability and the magnetic suspension force of superconductive block.
(2) Y is added 2baCuO 5opaque amount 0.1%, 0.5%, 0.8%, 1.5%, 2.0%, the WO of 3.0wt% 3powder, mixes, and is prepared into Y 2baCuO 5precursor powder.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.Being prepared into diameter is 20mm preparing YBCO superconducting blocks, and adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force to prepared single domain yttrium barium copper oxide superconductor respectively, and test result is in table 2 and Fig. 4.In the diagram, curve a is 0.1wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve b is 0.5wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve c is 0.8wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve d is 1.5wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve e is 2.0wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve f is 3.0wt%WO 3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping.
The magnetic suspension force test data of single domain yttrium barium copper oxide superconductor prepared by table 2 embodiment 4
From table 2 and Fig. 4, WO 3particle doping is followed successively by 0.1%, 0.5%, 0.8%, 1.5%, 2.0%, the magnetic suspension force of the preparing YBCO superconducting blocks of 3.0wt% is respectively 11.62N, 14.16N, 23.68N, 25.76N, 21.74N, 5.22N, as can be seen here, works as WO 3when particle doping is 1.5wt%, the magnetic suspension force of preparing YBCO superconducting blocks is up to 25.76N.

Claims (1)

1. a preparation method for single domain yttrium barium copper oxide superconductor, is characterized in that it is made up of following step:
(1) solid phase precursor powder is prepared
By Y 2o 3with BaCO 3, CuO powder be in molar ratio 1:1:1 ratio mixing, make Y with solid state reaction 2baCuO 5powder, gets Y 2baCuO 5powder joins ball mill, adds Y 2baCuO 5the WO of opaque amount 1.5% 3powder, mixes, and is prepared into solid phase precursor powder;
(2) liquid phase source powder is prepared
By Y 2o 3with BaCO 3, CuO be in molar ratio 1:4:6 mixing, sinter YBa into solid state reaction 2cu 3o 7-δpowder, BaCO 3be 1:1 in molar ratio with CuO, sinter BaCuO into solid state reaction 2powder, by YBa 2cu 3o 7-δpowder and CuO powder, BaCuO 2powder mixes for 1:2:3 in molar ratio, as liquid phase source powder;
0≤δ≤1 in above formula;
(3) solid phase pioneer's block and liquid phase block is suppressed
Get solid phase precursor powder and liquid phase source powder, being pressed into diameter is respectively the different solid phase pioneer block of 20mm thickness and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1:1.44%;
(4) back-up block is suppressed
By Y 2o 3powder is pressed into the briquet that diameter is 20mm, as back-up block;
(5) Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586g Nd 2o 3, 32.1727g BaCO 3, 12.9687g CuO powder mixing, Nd 2o 3with BaCO 3, CuO powder mol ratio be 1:1:1, make Nd with solid state reaction 2baCuO 5powder; Get 20.9895g Y 2o 3, 49.2386gBaCO 3, 29.7719g CuO powder mixing, Nd 2o 3with BaCO 3, CuO powder mol ratio be 1:4:6, make NdBa with solid state reaction 2cu 3o 7-δpowder; By Nd 2baCuO 5powder and NdBa 2cu 3o 7-δpowder is that 1:3 mixes according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method;
0≤δ≤1 in above formula;
(6) base substrate assembling and laying method
At Al 2o 3pad (6) upper surface to lower and on place MgO single-chip (5), back-up block (4), liquid phase block (3), solid phase pioneer block, Nd-Ba-Cu oxygen seed crystal blocks (1) successively;
(7) infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then be warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, be incubated 2 hours; Be cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block;
(8) oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 440 ~ 410 DEG C, slow cooling 200 hours, obtains single domain yttrium barium copper oxide superconductor.
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